Engineering Papers⌕ Search

SEARCH · Engineering Papers

Results for “Grain Boundary”

Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

Quote a phrase for an exact phrase match. Source license links do not imply unrestricted reuse.

At least 667 records · Page 37
All sourcesNASA NTRSDOE OSTI
DOE OSTI2025

Hydrogen and water interactions with CrMnFeCoNi alloy from density functional theory calculations

High entropy alloys (HEAs) are a promising class of materials with remarkable mechanical and catalytic properties. Among these, the quinary CrMnFeCoNi alloy (also called “Cantor alloy”) has attracted considerable attention given its thermodynamic stability and remarkable mechanical properties under different temperatures. Given that various degradation mechanisms involve multiple contaminants, such as hydrogen and water in hydrogen embrittlement and surface poisoning, respectively, understanding their interactions with the Cantor alloy is critical for its practical applications as structural, nuclear, or hydrogen storage material. In this work, we perform first-principles calculations based on Density Functional Theory (DFT) to investigate such interactions when considering various microstructures, including bulk materials and those containing certain defects, such as grain boundaries, stacking faults, and vacancies. We also employ Global Sensitivity Analysis to identify the importance of different factors in the stability of the impurities. We find that the accuracy of the H formation energy is significantly affected by spin polarization and chemical short-range order. The study also identifies a strong tendency for hydrogen interstitials to segregate to Σ5(210)/[001] symmetric tilt grain boundary, even when H concentrations are high, suggesting that a certain type of grain boundaries acts as H sinks within the alloy. Further, this result is reinforced by the low formation energy of vacancy-hydrogen complexes, which can contain multiple hydrogen atoms. Finally, the surface reactivity analysis reveals that the adsorption energy of oxygen and hydroxyl groups is highly sensitive to the specific metal atom involved in the binding, with a clear preference for chromium atoms, which could have implications for the alloy’s oxidation and corrosion behavior.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Validation of MFUEL Metal Fuel Performance Models of SAS4A/SASSYS-1

The fuel characterization models of SAS4A/SASSYS-1 (SAS) have recently been extended to include a new U-Pu-Zr metal fuel model, MFUEL. MFUEL is equipped with mechanistic physics based models to predict the pre-transient characterization and transient response of metal fuel, with emphasis on fuel melting, cladding failure, and the metal fuel’s impact on core reactivity. The MFUEL model will be available in the full version of SAS4A/SASSYS-1 5.7, which is scheduled to be released in June 2023. Fast reactor fuel pins that operated in EBR-II and FFTF with low smear density U-Zr and U-Pu-Zr metal fuels and irradiation resistant ferritic-martensitic cladding showed significant advantages in achieving high burnups and assuring inherent safety characteristics during anticipated transients, design basis events, and beyond design basis events. For safety analysis, a fuel performance model must be able to predict (1) Fuel pin mechanics and compositional and dimensional changes, (2) Clad failure, and (3) Fuel pin thermal resistance. Achieving these high level goals accurately is strongly related to the model performance of individual physical processes taking place within a fuel pin during its lifetime. Metal fuels typically operate above the mid-point temperature of melting during normal, as well as off-normal, conditions. At these elevated temperatures, the availability of thermal activation provides a driving force for various diffusional processes leading to complex phase transformations, micro-structure evolution, significant amounts of fuel swelling, interconnected porosity formation, excessive amounts of fission gas release, and fuel clad chemical interactions. Clad failure in fast reactors primarily occurs as a result of creep rupture augmented by clad wastage formation. The reaction is driven by thermal creep induced dislocation motion, grain boundary cavity nucleation, growth and breakup of grain boundaries. The high level complexity and limited available data requires introducing physics-based modeling approaches to gain extrapolation ability and sensitivity with respect to various conditions. The objective of this report is to perform validation of MFUEL using the experimental data for (1) Normal operation EBR-II fuel behavior, (2) Normal operation PHENIX fuel behavior, (3) HT9 Pressure tube ramp-and-hold creep rupture tests, (4) Whole Pin Furnace (WPF) creep strain, creep rupture and eutectic tests, (5) Fuel Behavior Test Apparatus (FBTA) eutectic tests, and (6) TREAT M5-7 OverPower tests up to clad failure. Section-2 includes a brief description of the MFUEL models. A detailed description of the MFUEL physics-based, semi-empirical models will be presented in the SAS V 5.7 theory manual. Section-3, 4, and 5 describes the validation effort for the pre-transient irradiation, furnace transients, and TREAT M-Series transients, respectively.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
NASA NTRS1972

Reversed creep deformation behavior of metals.

It is shown that the creep deformation resistance of a variety of metals is reduced by repeated reversed deformation at temperatures above 0.4 Tm, where Tm is the absolute melting temperature of each metal. The reduction of creep deformation resistance due to stress reversals is most prominent at approximately 0.5 Tm where the average creep rate may increase by as much as a factor of twenty due to 50-100 stress reversals. Metallographic studies show that the observed acceleration of creep at high temperatures is in part due to the enhancement of grain boundary sliding as a result of gradual grain boundary migration toward planes of maximum shear stress during reversed creep deformation.

Morrow, J.↗
NASA NTRS1995

Effect of microwave-enhanced superconductivity in YBa2Cu3O7 Bi-crystalline grain bounda ry weak-links

We have studied systematically the effect of microwave irradiation on the temperature dependent resistivity (R(I) and the current-voltage (I-V) characteristics of YBa2Gu3O(7 - x) (YBCO) bicrystalline grain boundary weak-links (GBWL's), with grain boundary of three different tilt angles. The superconducting transition temperature, T(sub c), has significant enhancement upon microwave irradiation. The microwave enhanced T(sub c) is increased as a function of incident microwave power, but limited to an optimum power level. The GBWL's of 45 deg tilt boundary has shown to be most sensitive to the microwave irradiation power, and the GBWL's of 36.8 deg tilt boundary has displayed a moderate response. In contrast, no enhancement of T(sub c) was observed in the GBWL's of 24 deg tilt boundary, as well as in the uniform films. Under the microwave irradiation, the R(T) dependent is hystertic as the transition taken from superconducting state to normal state and vice versa. Mechanisms associated with the redistribution of nonequilibrium quasiparticles under microwave irradiation are discussed.

Fu, C. M.↗
NASA NTRS2004

Thermo-Mechanical Properties of Super Sylramic SiC Fibers

Ceramic matrix composites (CMC) reinforced by Sic fibers, such as SiC/SiC, are targeted for application in hot-section components of advanced engines for aerospace propulsion and for electrical power generation. Two Super Sylramic Sic fiber types recently developed at NASA using the Sylramic fiber from COI Ceramics are candidates fof providing these components with improved thermal capability and improved performance. This paper reports on the state-of-the-art ability of these new fiber types to meet the key fiber requirements of these applications: high strength, high creep-rupture resistance, high environmental resistance, and high thermal conductivity. For example, creep-rupture tests performed at from 1350 to 1500 C under various environments to simulate CMC fabrication and service conditions show creep resistance in air improved -20 and -7 times in comparison to current Sylramic and Sylramic-iBN fiber types, respectively. This in turn resulted in an increase in fiber rupture life by up to two orders of magnitude. TEM and AES microscopic observations are presented to indicate that these improvements can be correlated with the replacement of weak grain boundary phases with stronger phases that hinder grain boundary sliding more effectively. SiC/SiC composite results are also provided to show the advantages of the Super Sylramic fiber types both for CMC fabrication and high temperature application.

Yun, H. M.↗
DOE OSTI2020

Ultrahigh temperature in situ transmission electron microscopy based bicrystal coble creep in zirconia I: Nanowire growth and interfacial diffusivity

This study demonstrates novel in situ transmission electron microscopy-based microscale single grain boundary Coble creep experiments used to grow nanowires through a solid-state process in cubic ZrO 2 between ≈ 1200 °C and ≈ 2100 °C. Experiments indicate Coble creep drives the formation of nanowires from asperity contacts during tensile displacement, which is confirmed by phase field simulations. The experiments also facilitate efficient measurement of grain boundary diffusivity and surface diffusivity. 10 mol% Sc 2 O 3 doped ZrO 2 is found to have a cation grain boundary diffusivity of $D_{gb} = (0.056 ± 0.05)exp (\frac{-380,000±41,000}{RT})m^2 s^{-1}$, and $D_s = (0.10 ± 0.27)exp(\frac{-380,000 ± 28,000}{RT}) m^2 s^{-1}$.

36 MATERIALS SCIENCE↗
DOE OSTI2024

How irradiation promotes intergranular stress corrosion crack initiation

Irradiation assisted stress corrosion cracking (IASCC) is a form of intergranular stress corrosion cracking that occurs in irradiated austenitic alloys. It requires an irradiated microstructure along with high temperature water and stress. The process is ubiquitous in that it occurs in a wide range of austenitic alloys and water chemistries, but only when the alloy is irradiated. Despite evidence of this degradation mode that dates back to the 1960s, the mechanism by which it occurs has remained elusive. Here, using high resolution electron backscattering detection to analyze local stress-strain states, high resolution transmission electron microscopy to identify grain boundary phases at crack tips, and decoupling the roles of stress and grain boundary oxidation, we are able to unfold the complexities of the phenomenon to reveal the mechanism by which IASCC occurs. The significance of the findings impacts the mechanical integrity of core components of both current and advanced nuclear reactor designs worldwide.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Accelerating Structure–Property Relationship Discovery with Multimodal Machine Learning and Self-Driving Microscopy

Microscopy combined with local spectroscopy is widely used to correlate nanoscale structure with functional properties in materials, but conventional measurements rely heavily on human-selected sampling locations and predefined targets, limiting data set diversity and the potential for discovery. Here, we present a framework that integrates autonomous microscopy with dual-novelty deep kernel learning (DN-DKL) for adaptive data acquisition and a dual variational autoencoder (VAE) for representation learning. DN-DKL actively guides the microscopy toward structurally and spectroscopically novel regions, enabling efficient collection of large spectral data sets. Dual-VAE embeds local structures and spectroscopic responses into a shared latent manifold that serves as a structure–property relationship map. We applied this framework for the investigation of halide perovskite films by using conductive atomic force microscopy. The results reveal distinct hysteresis behaviors that are linked to specific nanoscale structural motifs, including grain boundary junction points that show hysteresis under different bias conditions and asymmetric grain boundaries that suppress the charge transport. This framework establishes a general strategy that leverages the complementary strengths of self-driving microscopy, machine learning, and human expertise to accelerate scientific discovery in functional materials.

atomic force microscopy↗
DOE OSTI2023

High-temperature active oxidation of nanocrystalline silicon-carbide: A reactive force-field molecular dynamics study

Flexible woven SiC ceramics are prone to accelerated fiber embrittlement under high temperature oxidation in dynamic oxygen environments. The nanocrystalline structure of the constituent fibers impacts the reaction kinetics and phase transformations during active oxidation. However, fundamental understanding and quantification of grain boundary effects on oxidation behavior in nanocrystalline SiC remain elusive when temperatures exceed 1500 K. This study deploys large-scale molecular dynamics simulations with a reactive force-field to elucidate the complex roles of atomic oxygen reservoir conditions and grain size on oxidation kinetics and the nature of oxides produced in both monocrystalline and nanocrystalline 3C-SiC between 1100 K and 2000 K. The simulations with dynamically replenished oxygen provide good agreement with oxidation kinetics and activation energies for the monocrystalline Si(100) and C(100) orientations published in the available literature. This study reveals that, by contrast, nanocrystalline SiC samples exhibit two distinct oxidation kinetics with a transition point at 1500 K due to surface melting, which is supported by experimental evidence. The introduction of a grain-boundary network produces a two-fold decrease in oxidation activation energies compared to monocrystalline SiC below 1500 K. Above 1500 K, however, the activation energies rise substantially due to the formation of a liquid Si phase at the SiC/Si oxide interface. Further, it is shown that the stability of the interfacial liquid phase is promoted by incoherent grain boundaries in the crystalline SiC. These findings are important for the deployment of nanocrystalline SiC fibers in advanced thermal protection systems for high-temperature applications.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Examination Of IASCC In 304 Stainless Steel Core Shroud From A Commercial Boiling Water Reactor (BWR)

The 304 stainless steel core shroud and the accompanying weld material from a commercial boiling-water reactor (BWR) experienced an estimated dose of ~3.5 dpa neutron irradiation leading to irradiation-assisted stress corrosion cracking (IASCC). The resulting IASCC crack tips are examined with high-resolution analysis techniques, including scanning electron microscopy (SEM), scanning transmission electron microscopy (STEM), and atom probe tomography (APT), with select examples of directly correlated STEM/APT observations. Analytical observations reveal the crack morphology, composition, microstructure, and any associated corrosion-induced or radiation-induced segregation in the local metal grain boundaries ahead of the propagating SCC cracks. The observed oxide composition and structure were in-line with expectations, consisting of a Cr-rich inner oxide and a Fe-rich outer oxide, with the leading crack tip oxide being Cr-rich. In addition, the leading grain boundary exhibited typical radiation-induced segregation signatures that were largely unperturbed by the accompanying corrosion. Finally, the quantitative capabilities and limitations of STEM and APT in the context of corrosion fronts and grain boundary chemistry from the directly correlated measurements are discussed.

Olszta, Matthew J.↗
DOE OSTI2022

Inorganic cesium lead mixed halide based perovskite solar materials modified with functional silver iodide

Inorganic CsPbIBr 2 perovskites have recently attracted enormous attention as a viable alternative material for optoelectronic applications due to their higher efficiency, thermal stability, suitable bandgap, and proper optical absorption. However, the CsPbIBr 2 perovskite films fabricated using a one-step deposition technique is usually comprised of small grain size with a large number of grain boundaries and compositional defects. In this work, silver iodide (AgI) will be incorporated as an additive into the CsPbIBr 2 perovskite precursor solution to prepare the unique perovskite CsI(PbBr 2 ) 1-x (AgI) x . The AgI additive in the precursor solution works as a nucleation promoter which will help the perovskite to grow and merge into a continuous film with reduced defects. With detailed characterizations, we found that incorporating AgI additive resulted in a uniform perovskite film with fewer grain boundaries, increased grain size, crystallinity, optical absorption while decreasing carrier recombination and trap density. Using the AgI in an optimum amount, we fabricated CsPbIBr 2 perovskite solar cells (PSCs) with a simple structure and achieved a power conversion efficiency (PCE) of 7.2% with a reduced hysteresis index. This work offers an alternative approach towards preparing high-quality CsPbIBr 2 perovskite films for solar cells with higher stability and other optoelectronic applications.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
NASA NTRS1987

The role of boron in ductilizing Ni3Al

Ductilization of Ni3Al at room temperature by microalloying with boron has been primarily attributed to the increased grain boundary cohesion in the presence of boron. However, another aspect of the role played by boron in ductilizing Ni3Al is revealed when the Hall-Petch relationships for Ni3Al and B-doped Ni3Al are compared. A shallower slope for the B-doped Ni3Al compared to that for Ni3Al indicates a reduced resistance to slip propagation across grain boundaries, and therefore reduced stress concentration at boundaries, in the presence of boron. This comparison of Hall-Petch relationships was carried out by generating data for powder processed B-doped Ni3Al at various grain sizes and by compiling data for Ni3Al from the literature. In addition, the room temperature fracture of B-doped Ni3Al has been shown to initiate along certain grain boundaries. The fracture eventually occurs by transgranular ductile tearing.

Vedula, K.↗
DOE OSTI2025

Rapid Bayesian High Entropy Alloy Designs Fabricated via Wire Arc Additive Manufacturing

Purpose: This project seeks to demonstrate a new high-throughput (rapid) alloy design technique applied to creating new high entropy alloys (HEAs) for extreme environments. High entropy alloys shift the design paradigm from being focused on a single principal element (e.g. nickel-based alloys) to target alloys that include high atomic fractions (X >10%) of multiple elements. These HEA materials can exhibit sluggish diffusion and enhanced corrosion resistance, ideal for potential applications in advanced ultra supercritical (A-USC) steam cycles for power generation. Scope: The addition of multiple elements in high atomic fractions creates an enormous design space that cannot easily be investigated by traditional material design strategies such as designed of experiments (DOE). This project utilizes a Bayesian machine learning algorithm that has been modified to work with calculation of phase diagrams (CALPHAD) software. This Bayesian algorithm reduces manual inputs and increase the likelihood of achieving an optimal solution. Compositional inputs to this algorithm will be assessed using existing material property models for high temperature strength and corrosion resistance. The target for alloy performance will be a 15% (~100 ⁰C) increase in allowable service temperature beyond heat-resistant stainless steels while maintaining or improving alloy cost and corrosion resistance. Haynes 230 was selected as a baseline, which is 57 wt% Ni with 22 wt% Cr 14 wt% W, and 2 wt% Mo as solid solution strengtheners. In addition to rapid design via Bayesian machine learning, the alloys were rapidly fabricated using a multi-wire arc additive manufacturing (mWAAM) technique which allows for precise control of alloy composition and assessing of alloy design “windows” to study composition effects. Build speeds for wire-arc additive processes are among the highest for additive technologies enabling rapid and reliable sample fabrication when compared to conventional methods such as arc button melting. The mWAAM samples will be rapidly characterized via instrumented indentation for room temperature modulus and strength and for elevated temperature strength via hot hardness tests. After being screened with hardness testing, potential alloys will be further evaluated with conventional microscopy techniques including scanning electron microscopy (SEM) and transmission electron microscopy (TEM) to assess agreement with modeling results. The most promising compositions will also be evaluated by printing full sized tensile specimens for mechanical behavior tests at elevated temperatures. Results: Bayesian machine learning of a single performance function was initially used to optimize five performance metrics: 1) single phase stability, 2) yield strength, 3) creep resistance (low diffusion coefficient), 4) freezing range (weldability), and 5) material cost. The single performance function was suboptimal as assumptions had to be made about the results while formulating the optimization. A goal-oriented Bayesian optimization strategy (Hanaoka, 2021) was implemented with CALPHAD for use with the five metrics above. This multi-objective Bayesian optimization (MOBO) enabled the design of NiCrCoFe alloys with V and W additions. A base composition of NiCoCr was selected as Ni provides a stable FCC matrix, Cr aids corrosion/oxidation resistance, and Co is a solid-solutions strengthener that also improves creep by increasing the activation energy. Fe helps reduce diffusion coefficients and cost. Finally, V and W were selected for their reasonable solubility and high atomic misfit to aid in solid solution strengthening. Cracking of the mWAAM specimens was an early issue, and the Easton solidification cracking model (Easton et al., 2014a) was selected for addition to the MOBO function. High performing alloys fabricated by mWAAM included Ni 28 Cr 25 Co 26 Fe 15 V 8 and Ni 62 Cr 18 Co 1 Fe 3 W 15 . It was observed that even after adapting the mWAAM process for W, the W did not fully dissolve. To fully evaluate the Ni 62 Cr 18 Co 1 Fe 3 W 15 composition, a cored wire (80-20 NiCr sheath/powder core) was manufactured and printed via WAAM, and HIP’ing was utilized to homogenize and densify the printed alloy. The V and W alloys produced met metrics 1 (solid solution), 4 (solidification cracking), and 5 (cost). However, an unmodeled mechanism of thermal stress cracking was identified in the WAAM produced materials, perhaps exacerbated by the lack of grain boundary strengthening elements (B, C). Conclusions & Recommendations: A high-throughput (rapid) alloy design technique was applied to designing and manufacturing new high entropy alloys (HEAs) for extreme environments utilizing MOBO and mWAAM. The developed process was rapid and effective in addressing the mechanisms included in the model. The lack of grain boundary strengthening element additions (e.g., B, C) was a simplification that likely produced thermal stress cracking that turned into a large part of the investigation. Additions on the order of 0.005 wt% B and 0.05 wt% C likely would have minimized thermal stress grain boundary cracking. Overall, the high throughput design strategy is promising for rapid design of metrics-driven alloys for advanced ultra supercritical (A-USC) steam cycles for power generation. The MOBO and mWAAM process could be commercialized to accelerate metrics-driven alloy design. In addition, the cored-wire process utilized for scale-up is a promising high-volume process for WAAM alloy development and scale-up.

36 MATERIALS SCIENCE↗
DOE OSTI2020

He ion irradiation response of a gradient T91 steel

Metallic materials with a gradient microstructure usually exhibit excellent mechanical properties. How- ever, the radiation response of gradient structural materials is less well understood. In this work, room- temperature He ion irradiation up to ~4.5 dpa with ~10 at% He injection was performed on a gradient T91 steel processed by surface severe plastic deformation. In comparison to the coarse-grained ferritic T91, the gradient T91 with the nanocrystalline layers shows improved radiation tolerance in terms of less bubble swelling and radiation hardening. Additionally, bubble distribution along grain boundaries depends on misorientation angle suggesting a strong capacity of non-equilibrium grain boundaries in storing He atoms. The present study provides insight into the design of radiation tolerant gradient steels for nuclear industry applications.

36 MATERIALS SCIENCE↗
NASA NTRS2020

Microstructure and Hardness of 57Ni –40Ti –3Hf (wt.%)

Ni-rich NiTiHf (57 wt.% Ni – 40 wt.% Ti – 3 wt.% Hf) is an intermetallic material that is superelastic, corrosion resistant and hardenable through relatively simple heat treatment procedures. The composition, microstructure and hardness of two separate lots of Ni-rich NiTiHf were investigated. The measured compositions for both lots were nominal, with total impurities in each of less than 0.01 wt%. The average grain sizes were 28.0µm and 26.4µm for the two lots. In its annealed condition (1,050°C × 48h/furnace cool to room temperature), the microstructure consisted of a B2 (cubic) NiTiHf parent phase with abundant Ni4Ti3 precipitates and a few TiC inclusions. The grain boundaries were decorated with HfO2 particles and metastable Ni3Ti2 precipitates that were cubic in structure. The average hardness varied from approximately 470HV to 490HV for the two lots. The hardened (annealed then 900°C × 2h/water quench to room temperature) microstructure consisted of a B2 NiTiHf parent phase with no precipitates, HfO2 decorating the grain boundaries and some TiC inclusions. The average hardness in this heat treatment condition was approximately 580HV for both lots. The aged (hardened then 400°C × 30min/water quench to room temperature) microstructure consisted of a B2 NiTiHf parent phase containing a high density of very fine Ni4Ti3 precipitate phase, HfO2 decorating the grain boundaries and some TiC inclusions. For each lot, the average hardness decreased slightly after aging as compared to the hardened heat treatment condition. This report is expected to serve as a reference for a forthcoming Materials Specification for the use of Ni-rich NiTiHf in flight hardware.

intermetallics, compositional analysis, Vickers ha↗
DOE OSTI2025

Laser repair welding of irradiated alloy 182

Welding repair of irradiated nickel-based alloys, such as Alloy 182, poses a significant challenge due to helium-induced cracking (HeIC) and grain boundary degradation (GBD) in the heat affected zone, driven by helium accumulation at grain boundaries and welding-induced tensile stresses. This study investigates the weldability of irradiated Alloy 182 up to 15 wppm doped boron using both conventional laser welding and the Auxiliary Beam Stress Improved (ABSI) laser welding technique. While HeIC was observed at the weld toe of the entry pass in both methods due to the higher effective heat input associated with the initial pass directly on the base metal, no additional cracking occurred elsewhere, even at elevated helium concentrations. Optical and scanning electron microscopy analysis revealed that the ABSI technique, which introduces additional compressive stresses to counteract solidification-induced tensile stresses, significantly reduced GBD formation, lowering its total count from 1,230 to 339 and decreasing both average and maximum GBD lengths. In conclusion, these results demonstrate that the ABSI technique is a promising approach to mitigate helium-induced damage and improve the weldability of irradiated Alloy 182, offering a viable solution for structural repairs for long-term operation of existing nuclear reactors.

grain boundary degradation↗
NASA NTRS2010

A Compendium of Scale Surface Microstructures: Ni(pt)al Coatings Oxidized at 1150 C for 2000 1-h Cycles

The surface structure of scales formed on Ni(Pt)Al coatings was characterized by SEM/EDS/BSE in plan view. Two nominally identical {100} samples of aluminide coated CMSX4 single crystal were oxidized at 1150 C for 2000 1-h cycles and were found to produce somewhat disparate behavior. One sample, with less propensity for coating grain boundary ridge deformation, presented primarily alpha-Al2O3 scale structures, with minimal weight loss and spallation. The original scale structure, still retained over most of the sample, consisted of the classic theta-alpha transformation-induced ridge network structure, with approx. 25 nm crystallographic steps and terraces indicative of surface rearrangement to low energy alumina planes. The scale grain boundary ridges were often decorated with a fine, uniform distribution of (Hf,Ti)O2 particles. Another sample, producing steady state weight losses, exhibited much interfacial spallation and a complex assortment of different structures. Broad areas of interfacial spalling, crystallographically-faceted (Ni,Co)(Al,Cr)2O4 spinel, with an alpha-Al2O3 base scale, were the dominant features. Other regions exhibited nodular spinel grains, with fine or (Ta,Ti)-rich (rutile) particles decorating or interspersed with the spinel. While these features were consistent with a coating that presented more deformation at extruded grain boundaries, the root cause of the different behavior between the duplicate samples could not be conclusively identified.

Smialek, James L.↗
DOE OSTI2020

Report on partially complete post-irradiation-examination of the INL samples

Ferritic-martensitic steels (NF616 and T91), and austenitic stainless steel 800H and its Grain Boundary Engineering (GBE)-treated version 800H-TMP (ThermoMechanical Processing) were irradiated in the Advanced Test Reactor (ATR) at Idaho National Laboratory (INL) and their microstructures and mechanical properties were characterized. Ferritic-martensitic steels were irradiated up to 8.16 dpa in the irradiation temperatures ranging from 241 °C to 447.5 °C. Selected 800H and 800H-TMP samples were also irradiated up to 9.12 dpa at 359°C to 431°C. Vickers hardness measurement, fractography, and microstructural characterization were performed on the selected samples in the LAMDA lab. Radiation-induced hardening of NF616 and T91 was observed in the hardness measurements which show ~37% to ~65% increases, depending on irradiation dose and irradiation temperature. Within the irradiation conditions studied in this work, samples with a higher dose had a higher hardness. All the tested alloy 800H and 800H-TMP in this work showed irradiation-hardening by ~96±7% to ~152±10%. Alloy 800HTMP tended to have slightly smaller irradiation-hardening than alloy 800H. The fractography of NF616 samples D2 (2.96 dpa at 291.5°C), D4 (5.91 dpa at 359°C), and D6 (8.16 dpa at 431°C) indicated loss of ductility with negligible necking for the sample D2, yet obvious ductile failure for samples D4 and D6. Fractography of alloy 800H samples N4 (7.27 dpa at 359°C), N5 (3.9 dpa at 451.5°C), and N6 (9.01 dpa at 431°C), and alloy 800H-TMP samples P4 (7.36 dpa at 359°C), P5 (3.95 dpa at 451.5°C), and P6 (9.12 dpa at 431°C) indicated that all samples failed in a ductile mode, with obvious necking. Dimples were observed where large Ti-containing particles were observed for the samples. TEM characterization was performed on alloy 800H (N4, N5, N6) and 800H-TMP (P4, P5 and P6). Accumulation of M23C6 precipitates at grain boundaries was observed in all samples, and the presence of Ti(C,N) precipitates at grain boundaries and in the matrix was observed in alloy 800H-TMP. M23C6 precipitates were found to have the cube-on-cube orientation relationship with the matrix. In addition, nanoscale Si-rich clusters were observed in the matrix of all samples. Atom probe tomography was conducted on the same samples, and their results are being analyzed to be integrated with the TEM results for a confident description of the clustering behavior. Due to the low irradiation temperature (up to 451.5°C), dislocation loops formed in all samples, with the density and the average size of dislocation loops in the order of 1022 – 1023 m-3 and 11.7 – 15.9 nm, respectively. The loop densities in alloy 800H were higher than that in alloy 800H-TMP under the same irradiation conditions. Further systematic data analyses, together with some complementary experiments, will be pursued for these samples to foster peer-reviewed journal article publications.

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗