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At least 433 records · Page 24

Automated Grain Boundary (GB) Segmentation and Microstructural Analysis in 347H Stainless Steel Using Deep Learning and Multimodal Microscopy

Austenitic 347H stainless steel offers superior mechanical properties and corrosion resistance required for extreme operating conditions such as high temperature. The change in microstructure due to composition and process variations is expected to impact material properties. Identifying microstructural features such as grain boundaries thus becomes an important task in the process-microstructure-properties loop. Applying convolutional neural network (CNN)-based deep learning models is a powerful technique to detect features from material micrographs in an automated manner. In contrast to microstructural classification, supervised CNN models for segmentation tasks require pixel-wise annotation labels. However, manual labeling of the images for the segmentation task poses a major bottleneck for generating training data and labels in a reliable and reproducible way within a reasonable timeframe. Microstructural characterization especially needs to be expedited for faster material discovery by changing alloy compositions. Here, in this study, we attempt to overcome such limitations by utilizing multimodal microscopy to generate labels directly instead of manual labeling. We combine scanning electron microscopy images of 347H stainless steel as training data and electron backscatter diffraction micrographs as pixel-wise labels for grain boundary detection as a semantic segmentation task. The viability of our method is evaluated by considering a set of deep CNN architectures. We demonstrate that despite producing instrumentation drift during data collection between two modes of microscopy, this method performs comparably to similar segmentation tasks that used manual labeling. Additionally, we find that naïve pixel-wise segmentation results in small gaps and missing boundaries in the predicted grain boundary map. By incorporating topological information during model training, the connectivity of the grain boundary network and segmentation performance is improved. Finally, our approach is validated by accurate computation on downstream tasks of predicting the underlying grain morphology distributions which are the ultimate quantities of interest for microstructural characterization.

36 MATERIALS SCIENCE↗

Ab-initio predictions of phase stability, electronic structure, and optical properties of (0001)-MAX surfaces in M 2 AC (M = Cr, Zr, Hf; A = Al, Ga)

In this work, we report MAX phases' surface properties, which are essential for thin-film technology due to their excellent resistance to high-temperature oxidation, corrosion, and wear. The surface stability, electronic, and optical properties of 0001-surfaces in M 2 AC (M = Zr, Hf, Cr; A = Al, Ga) are investigated and compared with their bulk counterparts. The interplay between chemical bonding and charge distribution is discussed from electronic structure, including the Fermi surfaces. Four possible (0001)-terminated surfaces are considered by breaking M - C and M-A bonds in which cleavage energy of M - C is higher than M-A. The Cr–Al bond in Cr 2 AlC is stronger than other M-A bonds. The charge density of valance A-p electrons redistributes in the surface area, distinct from that of the bulk. The A- and M(C)-terminated (0001)-surfaces are the most stable and energetically favorable terminations due to lower surface energies. The optical properties of the most stable (0001)-surfaces were also investigated to understand the dielectric and photoconductive behavior in the (0001)-terminated surfaces of M 2 AC.

36 MATERIALS SCIENCE↗

High-temperature ferromagnetism in Cr 1+x Pt 5-x P

In this work, we present the growth and basic magnetic and transport properties of Cr 1+x Pt 5-x P. We show that single crystals can readily be grown from a high-temperature solution created by adding dilute quantities of Cr to Pt-P based melts. Like other 1-5-1 compounds, Cr 1+x Pt 5-x P adopts a tetragonal P4/mmm, structure composed facesharing CrPts like slabs that are broken up along the c-axis by sheets of P atoms. EDS and X-ray diffraction measurements both suggest Cr 1+x Pt 5-x P has mixed occupancy between Cr and Pt atoms, similar to what is found in the closely related compound CrPtg, giving real compositions of Cr 1.5 Pt 4.5 P (x = 0.5). We report that Cr 1.5 Pt 4.5 P orders ferromagnetically at T c = 464.5 K with a saturated moment of ≈ 2.1 μs/Cr at 1.8 K. Likely owing to the strong spin-orbit coupling associated with the large quantity of high Z, Pt atoms, Cr 1.5 Pt 4.5 P has exceptionally strong planar anisotropy with estimated anisotropy fields of 345 kOe and 220 kOe at 1.8 K and 300 K respectively. The resistance of Cr 1.5 Pt 4.5 P has a metallic temperature dependence with relatively weak magnetoresistance. Electronic band structure calculations show that CrPt 5 P has a large peak in the density of states near the Fermi level which is split into spin majority and minority bands in the ferromagnetic state. Furthermore, the calculations suggest substantial hybridization between Cr-3d and Pt-5d states near the Fermi level, in agreement with the experimentally measured anisotropy.

36 MATERIALS SCIENCE↗

Anisotropic optical and magnetic response in self-assembled TiN–CoFe 2 nanocomposites

Transition metal nitrides (e.g., TiN) have shown tremendous promise in optical metamaterials for nanophotonic devices due to their plasmonic properties comparable to noble metals and superior high temperature stability. Vertically aligned nanocomposites (VANs) offer a great platform for combining two dissimilar functional materials with a one-step deposition technique toward multifunctionality integration and strong structural/property anisotropy. Here, we report a two-phase nanocomposite design combining ferromagnetic CoFe 2 nanosheets in the plasmonic TiN matrix as a new hybrid plasmonic metamaterial. The hybrid metamaterials exhibit anisotropic optical and magnetic responses, as well as a pronounced magneto-optical coupling response evidenced by Magneto-optic Kerr Effect measurement, owing to the novel vertically aligned structure. This work demonstrates a new TiN-based metamaterial with anisotropic properties and multifunctionality toward light polarization modulation, optical switching, and integrated optics.

36 MATERIALS SCIENCE↗

Antiferromagnet to ferromagnet crossover driven by nonmagnetic Co doping in heavy-fermion YbRh 3 Si 7

YbRh 3 ⁢Si 7 is a heavy fermion compound that stands out among Yb-based heavy fermions, with its relatively high magnetic ordering temperature and large Yb-Yb distance. To investigate the origin of the magnetic properties in this compound, we synthesized Co doped YbRh 3⁢ Si 7 , achieving a record-high ferromagnetic ordering temperature T C =15.6K, only limited by the Co solubility of 20%. Furthermore, we find a crossover from antiferromagnetic to ferromagnetic order with Co doping. Additionally, the specific heat and magnetotransport measurements show heavy fermion behavior and the persistence of Kondo latticelike behavior in the Yb⁢(Rh 1-x Co x ) 3⁢ Si 7 series.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Elevated temperature nanoscratch of Inconel 617 Superalloy

Inconel 617 superalloy is a main candidate to be used for mechanical and tribo-components in high temperature helium-cooled reactors. Recent findings show that it grows a unique surface oxide, especially under high temperature helium with distinct wear, friction, and contact properties. Here, this study reports the elevated temperature nanoscratch behavior of Inconel 617 and further utilizes it to understand the effect of temperature on contact friction constituent contributors, adhesion and plowing at small scales. Inconel 617 is aged in high temperature helium, and consequently, the total kinetic friction coefficient of the alloy surface oxide is obtained in temperatures ranging from 25 °C to 400 °C. A finite element model is developed and validated based on the experimental results. The model is then utilized along with previously established techniques to determine the adhesion and plowing components of the friction coefficient. At small scale, the experimental results show that with increasing temperature the friction coefficient increases. It was inferred that this increase is mainly due to the increased contribution of plowing friction at high levels of deformation.

36 MATERIALS SCIENCE↗

Void formation during cyclic oxidation of oxide dispersion strengthened FeCrAl alloys

Here, oxide dispersion strengthened FeCrAl alloys are considered for various high-temperature applications due to their excellent mechanical properties and oxidation resistance, but void formation is a concern for component durability. Cyclic oxidation testing was conducted on alloy MA956 and PM2000 at 1100–1200ºC for durations of up to 10,000 h and the void content was determined from optical cross-sections by image analysis. At 1100ºC, 100 h cycle, the low void concentrations measured were consistent with two competing mechanisms proposed in the literature: coalescence of process-induced nano-voids and alloy sintering. At 1200ºC using 1 h cycles, the void concentration was much higher, reaching ~3% to 6% for specimens tested to breakaway oxidation. The void growth was attributed to the high oxidation rates and the annihilation of oxidation-induced vacancies at the surface of the process-induced voids.

36 MATERIALS SCIENCE↗

Development of a Laser Ultrasonics-based Approach for Rapid Screening of High Entropy Alloys

This project utilized a laser ultrasonic technique to systematically study temperature-induced evolution of material properties in a set of interrelated binary alloys and a high entropy alloy (HEA) fabricated using arc-melting and spark plasma sintering processes. This technique involved the use of a nanosecond duration, high-intensity pulsed laser to thermo-elastically generate ultrasonic waves that propagate in the bulk of the metal alloy. Sub-nanometer-scale displacements associated with the propagating bulk ultrasonic waves were detected along the epicenter on the opposite surface of the sample using a 1 GHz bandwidth photorefractive interferometer. Phase transformations and microstructural changes were inferred from the temperature-dependent trends in the bulk acoustic velocities and features in the ultrasonic epicentral waveforms measured in the binary alloys. These inferences were then correlated with electron/optical microscopy observations and predictions using calculations of phase diagrams (CALPHAD). The results showed that the laser-generated ultrasonic pulses were strongly influenced by changes in material microstructure and could accurately track thermally driven phase transformations and detect the presence of microscale heterogeneities (grain boundaries, dendritic structures, etc.) in the set of binary alloy samples. The measurement approach was then applied to a quinary HEA sample for estimating phase transition temperature and determining microstructural heterogeneity. The rapid, non-contact and non-destructive ultrasonic testing approach demonstrated here is amenable to high throughput combinatorial investigations that can be applied to graded composition HEAs produced using advanced manufacturing methods. When paired with atomistic simulations and CALPHAD modeling, this approach can overcome the bottlenecks faced by current material characterization methods in efficiently screening the vast discovery space of HEAs that spans over a hundred million unique quinary alloy compositions.

36 MATERIALS SCIENCE↗

Temperature-Dependent Carrier Extraction and the Effects of Excitons on Emission and Photovoltaic Performance in Cs0.05FA0.79MA0.16Pb(I0.83Br0.17)3 Solar Cells

The photovoltaic parameters of triple cation perovskite [Cs0.05FA0.79MA0.16Pb(I0.83Br0.17)3] solar cells are investigated focusing on the electro-optical properties and differences in performance at low and high temperatures. The signature of a parasitic barrier to carrier extraction is observed at low temperatures, which results in a loss of performance at T < 200 K. Intensity-dependent measurements indicate extraction across this parasitic interface is limited by a combination of the exciton binding energy and thermionic emission. However, the photovoltaic performance of the device is recovered at low intensity - where the photocarrier generation rate threshold is lower than the thermionic extraction rate. Loss of solar cell performance is also observed to be strongly correlated to an increase in photoluminescence intensity, indicating inhibited carrier extraction results in strong radiative recombination and that these systems do not appear to be limited by significant thermally activated non-radiative processes. Evidence of limited carrier extraction due to excitonic effects is also observed with a strong anti-correlation in photoluminescence and carrier extraction observed at lower temperatures.

barrier↗

Effect of Carbon Support Heat Treatment on the Performance of Ion-Pair High-Temperature PEM Fuel Cells

Heat treatment can significantly alter the physical and chemical properties of carbon supports, thereby influencing the performance of proton exchange membrane (PEM) fuel cells. This study explores how varying carbon heat treatment temperatures—from 1,000 °C to 2,200 °C—affect the structure and performance of platinum-based catalysts in high-temperature PEM fuel cells. Increasing the heat treatment temperature led to a notable decrease in surface area, along with increases in carbon grain size and hydrophobicity. Although the catalyst supported on carbon treated at 1,000 °C exhibited the highest catalyst activity, the MEA using carbon treated at 1,500 °C delivered the best overall fuel cell performance. This is attributed to an optimized balance between hydrophobicity and accessible surface area, which enhances water management and catalyst utilization. These findings underscore the importance of carbon support engineering in improving the efficiency of ion-pair high-temperature PEM fuel cells.

08 HYDROGEN↗

Low-temperature selective laser sintering 3D printing of PEEK-Nylon blends: Impact of thermal post-processing on mechanical properties and thermal stability

Herein, a high-performance polymer (HPP) (polyether ether ketone, PEEK) blended with a commercial low-temperature polymer (polyamide 12, PA-12) was fabricated using a low-temperature selective laser sintering (SLS) 3D printer. Different post-processing heat treatments were implemented after fabrication to tune the thermal and mechanical properties of printed blends. The specific mechanical modulus of the blend was increased up to 79% in comparison to printed PA-12 samples with heat treatment. Additionally, the thermal resistance of the treated blends greatly exceeded the properties observed using PA-12 alone. This research proposes a methodology to fabricate and engineer HPP using desktop SLS printers through a secondary lower melting temperature material and heat treatments.

36 MATERIALS SCIENCE↗

Searching for a route to synthesize in situ epitaxial Pr 2 Ir 2 O 7 thin films with thermodynamic methods

In situ growth of pyrochlore iridate thin films has been a long-standing challenge due to the low reactivity of Ir at low temperatures and the vaporization of volatile gas species such as IrO 3 (g) and IrO 2 (g) at high temperatures and high P O2 . To address this challenge, we combine thermodynamic analysis of the Pr-Ir-O 2 system with experimental results from the conventional physical vapor deposition (PVD) technique of co-sputtering. Our results indicate that only high growth temperatures yield films with crystallinity sufficient for utilizing and tailoring the desired topological electronic properties and the in situ synthesis of Pr 2 Ir 2 O 7 thin films is fettered by the inability to grow with P O2 on the order of 10 Torr at high temperatures, a limitation inherent to the PVD process. Thus, we suggest techniques capable of supplying high partial pressure of key species during deposition, in particular chemical vapor deposition (CVD), as a route to synthesis of Pr 2 Ir 2 O 7 .

Chemistry↗

Carrier recombination dynamics and temperature dependent optical properties of InAs–GaSb heterostructures

Heterostructures with two dissimilar materials could offer unprecedented properties if one can carefully synthesize these heterostructures with atomically smooth interfaces and reduced number of recombination centers. InAs/GaSb-based heterostructures have technological importance for long wavelength infrared photodetectors if one can synthesize these materials with high-optical quality and high-carrier lifetime. In this work, the InAs/GaSb heterostructures with a different number of heterointerfaces and growth conditions were grown by solid source molecular beam epitaxy using valved cracker sources for both arsenic and antimony. Precise control of growth parameters and shutter sequences enabled abrupt InAs/GaSb heterointerfaces, as supported by a high-resolution transmission electron microscopic study. The temperature and power-dependent optical properties by photoluminescence (PL) spectroscopic analysis of InAs/GaSb heterostructures with 4 and 28 heterointerfaces displayed donor to the acceptor and the exciton bound to complex defects (V Ga Ga Sb ) 0 . Since the optical transition in PL measurements serves to determine the quality of the material, and the observed excitonic transitions from these InAs/GaSb heterostructures is an indication of high-quality materials. The high-carrier lifetimes of 139 ns to 185 ns from InAs/GaSb heterostructures were measured using microwave photoconductivity decay (μ-PCD) technique at room temperature. The observed increase in carrier lifetime is due to the decreasing number of Ga-related carrier recombination centers or defect complexes. This is further supported by the PL spectroscopic study. In addition, the carrier lifetime with different injection levels is supported by Shockley–Read–Hall recombination. We report these InAs/GaSb heterostructures with high-optical quality and high-carrier lifetimes would offer a path for the development of high-performance infrared photodetectors.

36 MATERIALS SCIENCE↗

Synthesis, structure, linear and nonlinear optical properties of noncentrosymmetric quaternary diamond-like semiconductors, Cu 2 ZnGeSe 4 (CZGSe) and the novel Cu 4 ZnGe 2 Se 7

In this work, two quaternary diamond-like semiconductors (DLSs) in the Cu-Zn-Ge-Se system, the known Cu 2 ZnGeSe 4 (also referred to as CZGSe) and the new Cu 4 ZnGe 2 Se 7 , are compared in terms of their crystal structures, electronic structures and physicochemical properties. Both compounds were prepared by high-temperature, solid-state synthesis at 800 degrees C. Single crystal X-ray diffraction was used to determine the structure of Cu 4 ZnGe 2 Se 7 . The structures of both Cu 2 ZnGeSe 4 and Cu 4 ZnGe 2 Se 7 can be considered as derivatives of cubic diamond. Cu 4 ZnGe 2 Se 7 , with a reduced symmetry due to the cation ordering pattern, adopts the Cu 4 NiSi 2 S 7 structure type, with space group C2. The corner-sharing tetrahedra in Cu 4 ZnGe 2 Se 7 are slightly distorted because the charge for some of the S 2 - anions is not compensated by the first-nearest-neighbor cations. Rietveld refinements using synchrotron X-ray powder diffraction data were used to assess the phase purity of the samples and confirm the bulk structural behavior. Diffuse reflectance UV/Vis/NIR spectroscopy shows that Cu 2 ZnGeSe 4 and Cu 4 ZnGe 2 Se 7 have direct optical bandgaps of 1.38 and 0.91 eV, respectively. Electronic structure calculations implementing density functional theory confirm the direct bandgap for Cu 4 ZnGe 2 Se 7 , with a calculated value of 0.62 eV. Both compounds are air stable, thermally stable up to relatively high temperatures, undergo phase transitions and have wide windows of optical clarity. The Kurtz-Perry powder technique was used to determine the second harmonic generation (SHG) responses using a commercial AgGaSe 2 standard. While Cu 4 ZnGe 2 Se 7 displays a weak SHG response, Cu 2 ZnGeSe 4 exhibits a response that is greater than several benchmark materials, with a large SHG coefficient, χ (2) , of 43 ± 6 pm/V at λ = 2900 nm.

36 MATERIALS SCIENCE↗

Nuclear Structural Component Relevant Properties of Nickel-Based Alloys Produced via Additive Manufacturing

Idaho National Laboratory initiated examination of nickel-based alloys manufactured via three different additive manufacturing methods for potential applications in nuclear, high temperature structural components. The three methods analyzed included laser powder bed fusion, blown powder laser directed energy deposition, and wire-fed gas metal arc directed energy deposition. With the rapid push towards additive manufacturing, codes do not exist that definitively define what is or is not tolerable for each process and application, such as with conventional, wrought products. This report contains the initial work to understand possible manufacturing methods for high temperature alloys, and specifically, void formation, microstructure evolution, corrosion, and mechanical properties. To generate mechanical test data, specimens were tested irrespective of voids and microstructures were analyzed to better understand how to negate/improve these issues. The preliminary results showed major decreases in mechanical performance for material tested. Test specimens will continue to be produced to further improve each additive manufacturing processes, quantify void acceptance, and better understand the most suitable high temperature alloys receptive to additive manufacturing and high temperature nuclear applications.

36 MATERIALS SCIENCE↗

Research tool development for catalyst, catalyst/ionomer, and ionomer characterization above 100°C (CRADA Final Report)

There is a need to develop experimental tools that address the catalyst and ionomer interface under high-temperature proton-exchange-membrane (HT-PEM) operating conditions (dry, >100°C). These conditions mean traditional water-based measurements for membrane and ionomer properties are insufficient; new ex-situ techniques are required to address and characterize expected novel materials. In this project we develop a microelectrode cell for high temperature kinetics and gas transport properties and ex-situ ionomer thin-film characterization under these conditions. We use baseline Nafion and phosphoric-acid imbibed membranes as prototype materials for measuring the membrane/acid/ionomer systems with Pt microelectrodes and demonstrate feasibility of the tools.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Initial Developments in Modeling Graphite Behavior

Graphite is used in High Temperature Reactor designs as a moderator, reflector and core material responsible for protecting the fuel and maintaining structural stability. From a safety perspective, it is imperative to be able to predict how graphite will behave under reactor operating conditions which may compromise the core’s structural integrity or fuel’s safety performance. The following report summarizes recent modeling work undertaken at Idaho National Laboratory which focuses on graphite degradation behavior. One phenomenon which is explored in this report and can cause significant degradation to graphite properties is oxidation. Oxidation behavior in graphite is highly temperature dependent. At low temperatures, oxygen can fully penetrate a component and cause a homogeneous damage profile. At high temperatures, only the graphite near the surface of a component is affected. Understanding and modeling this temperature dependence is essential to predicting graphite behavior. In this report, three graphite models are discussed. The first model is used to investigate strength loss after low temperature oxidation. It does this by generating an approximate graphite microstructure then determining the required load to cause crack propagation. It has been shown that the model reproduces the quasi brittle stress versus strain relationship observed in graphite. Strength loss results from the model are shown to match experimental values. The second model investigates strength loss under high temperature oxidation conditions. This model is more applicable to full scale graphite components where the oxidation damage is often inhomogeneous throughout a component. The third model computes stresses in graphite under reactor conditions. Specifically, the model incorporates the effect of creep, irradiation dose, thermal strains, and oxidation in order to predict internal stresses in a component. All of these models are implemented in the Multiphysics Object-Oriented Simulation Environment (MOOSE), an open source, parallel finite element framework.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Codes and standards for ceramic composite core materials for High Temperature Reactor applications

Fiber-reinforced ceramic matrix composites are attractive for high-temperature nuclear applications due to excellent thermal and mechanical properties as well as reasonable-to-outstanding radiation resistance. Over the past 20 years, the use of ceramic matrix composite applications expanded to many commercial non-nuclear industries as fabrication and application of the technologies mature. The ASME Boiler Pressure Vessel Code, under Section III Division 5, provides the design and construction rules for High Temperature Reactor components. It published the first rules for ceramic matrix composites to be used for reactor core components. The rules lay out the quality requirements together with the design and materials criteria for the use and application of silicon carbide- and carbon-based matrix material technologies. As with the established graphite rules, the ceramic composite material rules are structured in Subsection HH (from Section III), that addresses the criteria for class SN nonmetallic core components. The code rules rely heavily on the development and publication of standards for composite specification, classification, and testing of mechanical, thermal, and other properties. These test methods are developed in ASTM Committee C28 on Advanced Ceramics, with a current focus on ceramic composite tubes. This article describes the detail of the composites code, the design methodology and similarities to the graphite code, the guidance for the development of specifications for ceramic composites (for nuclear applications) including recent standard developments, and it mentions the next steps to support licensing aspects by validating the code with benchmarking data.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗