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At least 325 records · Page 18

Micro-opto-mechanical devices and systems using epitaxial lift off

The integration of high quality, single crystal thin film gallium arsenide (GaAs) and indium phosphide (InP) based photonic and electronic materials and devices with host microstructures fabricated from materials such as silicon (Si), glass, and polymers will enable the fabrication of the next generation of micro-opto-mechanical systems (MOMS) and optoelectronic integrated circuits. Thin film semiconductor devices deposited onto arbitrary host substrates and structures create hybrid (more than one material) near-monolithic integrated systems which can be interconnected electrically using standard inexpensive microfabrication techniques such as vacuum metallization and photolithography. These integrated systems take advantage of the optical and electronic properties of compound semiconductor devices while still using host substrate materials such as silicon, polysilicon, glass and polymers in the microstructures. This type of materials optimization for specific tasks creates higher performance systems than those systems which must use trade-offs in device performance to integrate all of the function in a single material system. The low weight of these thin film devices also makes them attractive for integration with micromechanical devices which may have difficulty supporting and translating the full weight of a standard device. These thin film devices and integrated systems will be attractive for applications, however, only when the development of low cost, high yield fabrication and integration techniques makes their use economically feasible. In this paper, we discuss methods for alignment, selective deposition, and interconnection of thin film epitaxial GaAs and InP based devices onto host substrates and host microstructures.

Camperi-Ginestet, C.↗

Mechanical Test Results and Microstructural Characterization of the Harvested and Baseline Archival Zion RPV Materials

The decommissioning of the Zion Units 1 and 2 Nuclear Generating Station in Zion, Illinois, presented a unique opportunity for developing a better understanding of materials degradation and other issues associated with extending the lifetime of existing nuclear power plants (NPPs) beyond 60 years of service. In support of extended service and current operations of the US nuclear reactor fleet, the Oak Ridge National Laboratory (ORNL), through the Department of Energy (DOE), Office of Nuclear Energy, Light Water Reactor Sustainability (LWRS) Program, coordinated with Zion Solutions, LLC, a subsidiary of Energy Solutions (ES), the selective procurement of materials, structures, and components, from the decommissioned reactors including multiple segments of the Zion Unit 1 Reactor Pressure Vessel (RPV).

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

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

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

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Smoothed boundary method for simulating incompressible flow in complex geometries

Simulating flow through porous media with explicit considerations of complex microstructures is very challenging using conventional sharp-interface methods because of the difficulties in generating meshes conformal to complex geometries. In this work, a diffuse interface embedded boundary method known as the Smoothed Boundary Method (SBM) is utilized to facilitate simulations of fluid dynamics involving complex geometries. In diffuse-interface methods, the geometry is described by a domain parameter. The SBM allows the straightforward reformulation of the time-dependent Navier-Stokes equations in terms of this domain parameter, using only algebraic identities. Thus, enforcing the appropriate boundary conditions at the irregular embedded boundary is greatly simplified. Adaptive mesh refinement is used to increase the accuracy of the diffuse interface method by allowing thinner interfacial thickness to be used in the domain parameter. Here, the SBM-formulated Navier-Stokes equations are solved with the Finite Difference Method on refined mesh systems. Sharp-interface Finite Element Method simulations using the commercial software COMSOL on body-conforming meshes are also provided for comparison. Favorable agreement between the two methods is observed. Since it is no longer necessary for the mesh to conform to the complex geometry, the grid system for the SBM simulations can be generated rapidly and without additional manual interventions, making the entire simulation process more expedient.

36 MATERIALS SCIENCE↗

Irradiation of UC1+x kernels using the MiniFuel vehicle: Microstructure, phase analysis, and initial post-irradiation examination

Uranium carbide is a candidate fuel form for a wide range of advanced reactors, including larger Generation IV reactors as well as small modular reactors and microreactors. However, its commercial deployment timeline faces challenges via traditional qualification approaches. To address this issue, an accelerated fission rate irradiation test was performed to collect basic fuel performance data to inform fuel performance models and potential future integral tests. Hyperstoichiometric UC (UC1+x) kernels were irradiated in the High Flux Isotope Reactor using the MiniFuel irradiation vehicle. The test matrix spanned two temperature regimes (700 °C and 800 °C) and burnup levels (1.8 % FIMA and 2.8 % FIMA). Between 21 and 63 kernels were tested at each unique temperature and burnup condition. As-fabricated microstructural analysis revealed a multiphase composition with UC, UC2, UC2−y, and U-C-O bearing phases for the irradiated kernels. Following irradiation, fission gas release, swelling, and microstructures were analyzed. Measured fission gas release was below 5 % for all irradiation conditions, reaching a maximum at the highest temperature and burnup condition. A binary swelling response was observed; the lower burnup and temperature conditions resulted in negligible swelling, but the higher burnup and temperature conditions produced significant anisotropic swelling and densification in a subset of kernels. The basic microstructural exams of kernels following irradiation were not capable of showing a correlation between kernels that exhibited excessive swelling and those that did not. Characterization of a subset of samples using the Advanced Photon Source and more detailed microstructural examination of unirradiated kernels revealed that a subset of kernels contained very high UC2 phase fractions. The anomalous swelling response is hypothesized to have been driven by this chemical variation. The results of this irradiation highlight the potential of accelerated fission rate irradiation testing to explore such behaviors and inform the development of fuel specifications.

Adorno Lopes, Denise [ORNL] (ORCID:000900023705987↗

Experimental Insights into the Coupling of Methane Combustion and Steam Reforming in a Catalytic Plate Reactor in Transient Mode

The microstructured reactor concept is very promising technology to develop a compact reformer for distributed hydrogen generation. In this work, a catalytic plate reactor (CPR) is developed and investigated for the coupling of methane combustion (MC) and methane steam reforming (MSR) over Pt/Al 2 O 3 -coated microchannels in cocurrent and counter-current modes in transient experiments during start-up. A three-dimensional (3D) computational fluid dynamics (CFD) simulation shows uniform velocity and pressure distribution profiles in microchannels. For a channel velocity from 5.1 to 57.3 m/s in the combustor, the oxidation of methane is complete and self-sustainable without explosion, blow-off, or extinction; nevertheless, flashbacks are observed in counter-current mode. In the reformer, the maximum methane conversion is 84.9% in cocurrent mode, slightly higher than that of 80.2% in counter-current mode at a residence time of 33 ms, but at the cost of three times higher energy input in the combustor operating at ~1000 °C. Nitric oxide (NO) is not identified in combustion products, but nitrous oxide (N 2 O) is a function of coupling mode and forms significantly in cocurrent mode. Furthermore, this research would be helpful to establish the start-up strategy and environmental impact of compact reformers on a small scale.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

A Discussion of Strength Reduction Factor Development for Thermal Aging Effect on Nuclear Structural Alloys

In consideration of structural alloy property deterioration during long-term exposure to elevated temperatures, the yield and ultimate tensile strength reduction factors are provided in the Boiler and Pressure Vessel Code Section III for nuclear reactor component design and operation analysis. Because the Gen IV reactor requirement of 40 ~ 60 years of service life makes it difficult to acquire such long exposure test data for developing the reduction factors, they must be derived from test data with relatively short exposure by predictive methods considered to be reasonably reliable. A novel approach with a physically-based model has recently been proposed for application to development of reduction factors for 9Cr-1Mo-V. In the model, contributors to the tensile strength are first identified and related to definite microstructural features of the alloy, then some physically-based methods are employed to simulate the microstructural evolution, and finally the model is assembled with test-data-calibrated parameters to generate the yield and ultimate tensile strength reduction factors covering elevated temperature exposure for up to 57 years. The approach is undoubtedly a trailblazing development that will, if proven reliable, lead to a paradigm shift in predicting thermal aging behavior of many other alloys. Its debut application to Section III, however, concerns nuclear safety and naturally warrants objective, impartial, and thorough technical scrutiny. In the present paper, the novel and conventional approaches are discussed. Necessary improvements to the novel approach are recommended for its application to nuclear structural component design and analysis, and for its potential expanded use to other alloys.

Ren, Weiju↗

Non-Equilibrium Synthesis of Semiconductor Alloys for Energy Applications

This project explores the synthesis under equilibrium/non-equilibrium conditions of semiconductor alloys critical to SSL to impose top-down influence on the formation of atomic-scale microstructures. A plasma-enhanced MOCVD (PE-MOCVD) technique is employed, in which plasma generated within the low-pressure reactor environment introduces additional energy that is delivered to the gas-phase reactants and growth surface, allowing relatively low substrate temperatures to be maintained, rapidly switching the crystal-growth environment into a non-equilibrium state. The project coordinates on-going work at National Renewable Energy Laboratory (NREL) that addresses order/disorder Al x In 1-x P (AlInP) confinement structures, which are predicted to surpass the power-conversion efficiency of current materials used for red/amber LEDs as components of so-called color-mixed LEDs, which integrate multiple LEDs in a single device for improved color rendering. Ordering, phase separation, and strain relaxation are central to this technology. During growth, each spontaneous process could be suppressed or enhanced on demand by application of plasma as an additional handle. This technique could have broader applications to other energy technologies, such as photovoltaics.

14 SOLAR ENERGY↗

High-throughput, Ultra-fast Laser Sintering of Ceramics and AI Based Prediction on Processing-Microstructure-Property Relationships

We report high-throughput, ultra-fast laser sintering of alumina sample array and characterization of sample units’ microstructure and hardness, as a fast exploration of laser processing parameters, microstructure, and property. These experimental data were used to train machine-learning (ML) models. Accurate ML predictions were demonstrated for the processing-microstructure-property relationship, specifically in (1) prediction of the microstructure of alumina under arbitrary laser power and (2) prediction of the expected microstructure from the desired hardness. An independent neural network was developed and showed that ML-predicted microstructure had less than 10% error from real ones, in terms of projected hardness. To monitor the microstructure during laser sintering, we demonstrated an ML model that can instantaneously predict ceramic’s microstructure at the laser spot, based on the laser spot brightness. The ML model can generate more than 10 predictions per second, and the error in average grain size was less than 5% from the experimental observations.

36 MATERIALS SCIENCE↗

The continuing battle against defects in nickel-base superalloys

In the six decades since the identification of age hardenable nickel-base superalloys their compositions and microstructures have changed markedly. Current alloys are tailored for specific applications. Thus their microstructures are defined for that application. This paper briefly reviews the evolution of superalloy microstructures and comments on the appearance and implications of microstructural defects in high performance superalloys. It is seen that new alloys and proceses have generated new types of defects. Thus as the industry continues to develop new alloys and processes it must remain vigilant toward the identification and control of new types of defects.

Dreshfield, R. L.↗

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↗

Microstructural Characterization of Ion Irradiated ODS MA956 Alloy

Oxide Dispersion Strengthened (ODS) alloys are considered as promising nuclear materials for the next generation advanced nuclear reactors due to their improved elevated temperature mechanical properties and radiation damage resistance. MA956 is a commercial ODS alloy with superior oxidation resistance and creep strength at elevated temperatures. The improved properties for ODS alloys can be attributed to the presence of dispersed nanosized oxide particles. These oxide particles can act as barriers to dislocation motion and provide additional sinks and sites for point defect recombination. Hence, their stability can greatly affect the properties of the irradiated ODS alloys. Besides, irradiation will induce defects into the ODS alloys, and these defects can develop further as irradiation dose increases. Furthermore, the defects propagation can significantly undermine the mechanical properties of the bulk materials, resulting in irradiation hardening and lower ductility. Therefore, it is necessary to have a good understanding of the defect’s evolution with irradiation. Hence, efforts are ongoing to understand the effect of ion irradiation on ODS MA956 with emphasis on oxide particles and evolution of defects as a function of dose (2.5, 50 and 100 dpa).

07 ISOTOPE AND RADIATION SOURCES↗

Microstructural evolution of a silicon carbide-carbon coated nanostructured ferritic alloy composite during in-situ Kr ion irradiation at 300°C 450°C

This work focuses on irradiation behaviors of a novel silicon carbide and carbon coated nanostructured ferritic alloy (SiC-C@NFA) composite for potential applications as a cladding and structural material for next generation nuclear reactors. The SiC-C@NFA samples were irradiated with 1 MeV Kr ions up to 10 dpa at 300 and 450 °C. Microstructures and defect evolution were studied in-situ at the IVEM-Tandem facility at Argonne National Laboratory. The effects of ion irradiation on various phases such as α-ferrite matrix, (Fe,Cr) 7 C 3 , and (Ti,W)C precipitates were evaluated. The α-ferrite matrix showed a continuous increase in dislocation density along with spatial ordering of dislocation loops (or loop strings) at >5 dpa. The size of the dislocation loops at 450 °C was larger than that at 300 °C. The nucleation and growth of new (Ti,W)C precipitates in α-ferrite grains were enhanced with the ion dose at 450 °C. This study provides new insight into the irradiation resistance of the SiC-C@NFA system.

(FeCr)(7)C-3↗

Biopolymer-supramolecular polymer hybrids for photocatalytic hydrogen production

Solar generation of H 2 is a promising strategy for dense energy storage. Supramolecular polymers composed of chromophore amphiphile monomers containing perylene monoimide (PMI) have been reported as crystalline light-harvesting assemblies for aqueous H 2 -evolving catalysts. Gelation of these supramolecular polymers with multivalent ions creates hydrogels with high diffusivity but insufficient mechanical stability and catalyst retention for reusability. We report here on using sodium alginate (SA) biopolymer to both induce supramolecular polymerization of PMI and co-immobilize them with catalysts in a robust hydrogel with high diffusivity that can also be 3D-printed. Faster mass transfer was achieved by controlling the material macrostructure by reducing gel diameter and microstructure by reducing biopolymer loading. Optimized gels produce H 2 at rates rivaling solution-based PMI and generate H 2 for up to 6 days. The PMI assemblies in the SA matrix create a percolation network capable of bulk-electron transfer under illumination. These PMI–SA materials were then 3D-printed on conductive substrates to create 3D hydrogel photoelectrodes with optimized porosity. The design of these versatile hybrid materials was bioinspired by the soft matter environment of natural photosynthetic systems and opens the opportunity to carry out light-to-fuel conversion within soft matter with arbitrary shapes and particular local environments.

36 MATERIALS SCIENCE↗

Material Characterization of Grade 91 Steel Welds using, Micro-resolution Ultrasonic Imaging System

Grade 91 (9Cr-1Mo-V) steel is a common structural material for fossil-fuel fired and nuclear power plants because of its creep strength and oxidation resistance at high temperatures. In this research, we studied the feasibility of correlating the high-resolution images obtained from the immersion ultrasonic imaging technique to microstructure regions in Grade 91 steel plate weldments. The high-resolution ultrasonic images presented in this paper were generated using a 20-MHz focused transducer as the transmitter, and a laser vibrometer as the receiver in the through transmission configuration to produce longitudinal and shear waves. This nondestructive evaluation (NDE) method was used to identify the Fusion Zone (FZ), Heat-Affected Zone (HAZ), and Base Metal (BM) regions of Grade 91 cold metal transfer (CMT) and flux core arc welds (FCAW). The ultrasonic imaging results were analyzed using beam propagation amplitudes and homogeneity, which in turn were used to relate the different microstructure regions of the FCAW and CMT welded samples. With this study, we were able to identify highly susceptible microstructures in the weld that could potentially promote creep type failures.

20 FOSSIL-FUELED POWER PLANTS↗

High-Entropy Alloy R&D for Accelerator Beam Window Applications

High-Entropy Alloys are a class of novel material that can offer improved resistance to beam-induced radiation damage and thermal shock. Development of these new alloys to serve as beam windows in multi-megawatt accelerator target applications is ongoing at Fermilab. Currently we are investigating AlCoCrMnTiV alloy systems of 4-6 components for service as beam windows; these compositions are predicted by CALPHAD simulation to have a low density and single-phase BCC crystal structure. The microstructures of these systems are being studied by electron microscopy techniques such as energy dispersive X-ray spectroscopy (EDS) to determine elemental homogeneity and composition, electron backscatter diffraction (EBSD) to quantify grain structure and orientation, and transmission electron microscopy (TEM) to observe defect structures and precipitate formation; nanoindentation is used to probe microstructural mechanical properties. Initial bulk property characterization utilizes differential scanning calorimetry to quantify specific heat capacity (cp), dilatometry to determine the coefficient of thermal expansion (CTE), and time-domain thermoreflectance (TDTR) to measure thermal conductivity (K). A miniature tensile testing apparatus is also being developed to test tensile properties. Post-irradiation examination is currently ongoing for several of these compositions that have been irradiated by low-energy ions to damage levels and at a temperature relevant to beam window applications at future next-generation accelerator facilities. This talk will briefly describe the alloy design and synthesis before going into more depth covering microstructural pre-characterization, and post-irradiation examination results from low-energy ion irradiated specimens. This will be followed by the plans for alloy down selection and future prototypic proton irradiations.

43 PARTICLE ACCELERATORS↗

Iridescence from Total Internal Reflection at 3D Microscale Interfaces: Mechanistic Insights and Spectral Analysis

An experimental investigation and the optical modeling of the structural coloration produced from total internal reflection interference within 3D microstructures are described. Ray-tracing simulations coupled with color visualization and spectral analysis techniques are used to model, examine, and rationalize the iridescence generated for a range of microgeometries, including hemicylinders and truncated hemispheres, under varying illumination conditions. An approach to deconstruct the observed iridescence and complex far-field spectral features into its elementary components and systematically link them to ray trajectories that emanate from the illuminated microstructures is demonstrated. The results are compared with experiments, wherein microstructures are fabricated with methods such as chemical etching, multiphoton lithography, and grayscale lithography. Microstructure arrays patterned on surfaces with varying orientation and size lead to unique color-traveling optical effects and highlight opportunities for how total internal reflection interference can be used to create customizable reflective iridescence. The findings herein provide a robust conceptual framework for rationalizing this multibounce interference mechanism and establish approaches for characterizing and tailoring the optical and iridescent properties of microstructured surfaces.

36 MATERIALS SCIENCE↗

Microstructural Development of Directionally Solidified Hg(1-x)Zn(x)Se Alloys

Hg(1-x)Zn(x)Se alloys have been studied as an alternative to HgCdTe for the detection of electromagnetic radiation, because the shorter ZnSe and HgSe bonds were predicted to improve lattice stability. Previous studies showed that optical properties were stable with time and that the microhardness was higher than for HgTe based alloys. However, for this material to be commercially viable, compositional variations must be reduced, and the distribution of defects induced by the growth process must be understood. The basic structural properties of bulk materials were characterized, and dislocation etch pit densities were measured to determine whether the addition of Zn to the HgSe lattice reduced the potential for dislocation formation. Hg(0.9)Zn(0.1)Se alloys were directionally solidified using a modified Bridgman-Stockbarger method and in an applied magnetic field. Radial compositional variations were greatly reduced when solidification occurred in an applied magnetic field. The combination of a convex liquid-solid interface shape and a method for reduced wetting produced boules that were a single crystal after reaching full diameter. Observed surface features indicated ampoule wetting could be eliminated using a graphite getter. Microstructural characteristics were greatly improved over HgCdTe alloys, In six boules, a total of only one twin was observed, and no inclusions were found. A method for polishing and producing dislocation etch pits was developed for these alloys, revealing dislocation etch pit densities one to two orders of magnitude less than HgTe based alloys. A kink in the thermal profile during processing of one boule generated more dislocations than did lattice mismatch due to compositional variations. The results of this investigation indicate this alloy has improved microstructural properties and resistance to dislocation formation compared with similar II-VI alloys, and should be further investigated for the detection of electromagnetic radiation.

Cobb, S. D.↗