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At least 37 records · Page 2

Microstructural Analysis Across a Hybrid Inconel 718 Turbopump Inducer Following a Scheduled Heat Treatment Process

Additive Manufacturing (AM) provides a low-cost method to fabricate near net shape complex parts. In this study, a turbopump inducer was fabricated using blown powder direct energy deposition (DED) of Inconel 718 to form the fins on a wrought hub. By utilizing this combination process, more cost-effective methods are possible for complex parts. A series of heat treatments were applied to the assembly per ASTM F330.

Inconel 718

Porous Microstructure Analysis (PuMA) software

- Motivation and objectives - Overview of PuMA - Open-source release - Material properties computation - Artificial geometry generation - Property homogenization for anisotropic media - Fiber orientation - Conductivity - Elasticity - Permeability

homogenization

Development of Methods of Characterizing Coal in Its Plastic State

Coal in its plastic state (typically 400-460 C) was examined by the isothermal Gieseler plastometry of seven selected coals of widely varying plastic properties. Kinetic models were proposed for the isothermal plastometric curves. Plastic behavior was compared with a variety of laboratory analyses and characterizations of these coals, including classical coal analysis; mineral analysis; microstructural analysis (extractable fractions, surface area measurement, and petrographic analysis); and thermal analysis (thermogravimetric analysis, thermomechanical analysis, and differential scanning calorimetry). The phenomenon of a sharp, large, poorly reproducible exotherm in the differential scanning calorimetric analysis of coking coals was examined. Several coal extrudates show mineral distribution, organic maceral composition and overall calorific value to be little affected by 800 F extrusion. Volatile matter and plastic properties are moderately reduced, and the network structure (as gauged by extractables) appears to be slightly degraded in the extrusion process.

Lloyd, W. G.

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

Microstructure‐Informed Analysis Framework for Lattice Structures: Guiding Topology‐Material Synergy in Titanium Alloys

In this work we discuss a microstructure‐informed analysis framework for lattice structures that maps the material's microstructural response to guide topology selection and mechanical performance optimization. By coupling geometrical topology with intrinsic material behavior, we demonstrate how anisotropic microstructural response can inform the design of optimized lattice structures. To illustrate this concept, we focus on two distinct classes of titanium alloys: Ti5553 (Ti‐5Al‐5Mo‐5V‐3Cr wt%), which exhibits a predominantly ‐phase microstructure, and Ti64 (Ti‐6Al‐4V wt%), which features a dual‐phase structure. These alloys exhibit markedly different mechanical responses under multiaxial loading in “fully dense” solid form. The strut‐level stress analysis of these alloys reveals how specific microstructural characteristics can guide the selection of appropriate lattice topologies. Two representative lattice configurations, one stretching‐dominated and one bending‐dominated, are evaluated under identical loading conditions to explore how microstructure‐driven design can lead to topology choices that are better suited to accommodate shear or other critical local stress states, thereby enhancing mechanical performance. A strut‐level mechanics‐based analysis is performed to evaluate shear stress distribution and highlight the role of topology‐microstructure synergy and compatibility in determining overall lattice behavior. The findings emphasize the importance of designing structures that are both load‐aware and microstructure‐responsive, enabling more effective material utilization in advanced engineering applications.

36 MATERIALS SCIENCE

Revealing the microstructure of materials

The objectives are to demonstrate how the microstructure of materials may be revealed by abrasive polishing and chemical etching, and to illustrate how microstructural information is used to monitor manufacturing processes, provide in-depth inspection, and perform failure analysis. Microstructural analysis is the procedure used to reveal the internal microstructural details of a material or part by sectioning and polishing the cut surface so that it may be examined under a suitable microscope. A printed wiring board was selected as the test material because it contains both metals and nonmetals that have distinctive microstructures, and because this technique is used throughout the electronic industry as a key quality control tool. The three principle component materials in printed circuit boards are glass/epoxy laminates faced with copper foil; copper, deposited by both electroless and electrolytic plating; and tin/lead solder. Sample preparation, mounting, grinding, polishing, and examination and analysis are discussed.

Nelson, James A.

Mechanical Properties and Interfacial Bonding of Overmolded Polymer Composite Lattice Structures

This study investigates the mechanical properties and interfacial bonding of Polyamide 12 filled with Glass Fiber (PA12/GF) lattice structures overmolded with Nylon 66 (PA66) and Thermoplastic Polyurethane (TPU). The PA12/GF lattices, designed in Gyroid, Isotruss, and Octahedral geometries, were produced using the Selective Laser Sintering (SLS) technique. The thermal characteristics of both the lattice and overmolding materials were analyzed using Differential Scanning Calorimetry (DSC) and Thermogravimetric Analysis (TGA). The mechanical performance and interfacial bonding were evaluated through mechanical testing and microstructural analysis. The results indicate that overmolding improved flexural strength and impact resistance of the PA12/GF lattices. For instance, the plain PA12/GF Isotruss lattice exhibited a flexural strength of 15.5 MPa. By overmolding it with TPU the flexural strength increased by up to 137%, while PA66-overmolding resulted in an increase of 371%, achieving a flexural strength of 73 MPa. In terms of impact resistance, TPU-overmolding improved performance significantly, with an increase of 1800% (Gyroid) compared to the plain lattice. Microstructural analysis revealed good adhesion at the interface, especially when both the lattice and overmolding materials were thoroughly dried prior to the overmolding process to minimize interfacial porosity. This study highlights the potential of using overmolding to enhance lattice structures performance, offering lightweight and cost-efficient solutions for automotive applications.

Talabi, Isaac [ORNL] (ORCID:0000000340215594)

Inelastic Deformation of Metal Matrix Composites: Plasticity and Damage Mechanisms - Part 1

The deformation mechanisms of a Ti 15-3/SCS6 (SiC fiber) metal matrix composite (MMC) were investigated using a combination of mechanical measurements and microstructural analysis. The objectives were to evaluate the contributions of plasticity and damage to the overall inelastic response, and to confirm the mechanisms by rigorous microstructural evaluations. The results of room temperature experiments performed on 0 degree and 90 degree systems primarily are reported in this report. Results of experiments performed on other laminate systems and at high temperatures will be provided in a forthcoming report. Inelastic deformation of the 0 degree MMC (fibers parallel to load direction) was dominated by the plasticity of the matrix. In contrast, inelastic deformations of the 90 degree composite (fibers perpendicular to loading direction) occurred by both damage and plasticity. The predictions of a continuum elastic plastic model were compared with experimental data. The model was adequate for predicting the 0 degree response; however, it was inadequate for predicting the 90 degree response largely because it neglected damage. The importance of validating constitutive models using a combination of mechanical measurements and microstructural analysis is pointed out. The deformation mechanisms, and the likely sequence of events associated with the inelastic deformation of MMCs, are indicated in this paper.

Majumdar, B. S.

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

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

36 MATERIALS SCIENCE

Microscopy and microstructure of Shuttle thermal protection system materials

Examples of the contribution of microstructural analysis to the development of the Space Shuttle tile insulation system are presented, with photographic examples of the scanning electron microscope (SEM) investigations. After the basic thermal protection system materials had been selected, it was neccessary to analyze the mechanical responses of the combined materials; which included: (1) the polymer strain isolation pad (SIP), (2) the room temperature-vulcanizing silicone rubber bond, (RTV), and (3) rigid ceramic fiber reusable surface insulation (RSI). Microstructural analysis was used to provide information on deformation and fracture mechanisms, load transfer mechanisms, and structural alterations occurring before final failure. Both quantitative and qualitative information was obtained in the open, three-dimensional fibrous structures of the ceramic tiles by means of novel techniques of encapsulation and dissolution.

Newquist, C. W.

Survey of baffle plate samples, specimen machining, and hydrogen measurements

This report outlines preliminary results on the survey and characterization of irradiated baffle plate, baffle former, and flux thimble tube specimens as part of the ongoing investigation into irradiation-induced embrittlement in austenitic stainless steels at ambient (room temperature) conditions. The specimens originated from commercial pressurized water reactor (PWR) components, covering displacement damage doses ranging from approximately 0.065 to 75 dpa. Initial scanning electron microscopy (SEM) surveys revealed that specimen surfaces exhibited fine machining marks and in-service-formed oxide layers on the side surfaces of the analyzed specimens. The oxide layers revealed specific features resembling localized "pitting-like" corrosion. An additional set of specimens representing in-service oxidation is being preserved for future microstructure analysis work. As believed, this will provide additional insights into long-term material degradation in PRWs. Specimen machining challenges emerged due to a complex failure of the electric discharge machining (EDM) system located in hot area. Despite partial restoration, issues persist with the EDM’s secondary power supply, necessitating the exploration of alternative EDM or computer numerical control (CNC) machining approaches to facilitate tensile specimen preparation. Currently, low speed saw cutting is in progress to prepare specimens for hydrogen measurements and general microstructure analysis. The near-term goals include completing tensile specimen machining for advanced mechanical testing and characterizing fracture mechanisms, and stress-corrosion cracking testing, ultimately aiming to identify and mitigate the ambient-condition intergranular cracking through targeted post-irradiation annealing strategies.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS

3D Printed Ceramic Reinforced Polymer Composites Microstructure and Mechanical Properties

In Fused Filament Fabrication (FFF) 3D printing a part is made by extruding material layer by layer. Benefits of FFF are the ability to print complex shapes quickly and at a lower cost compared to other manufacturing methods. In this work, filaments composed of either silicon carbide (SiC) or zirconium silicate ceramic particulates in a polylactic-acid (PLA) matrix were used to print specimens for microstructural analysis and mechanical testing. Pure PLA samples were also printed and tested as a baseline for comparison. A Design of Experiments approach was used to test the interactions between three different parameters and their effect on ultimate strength, Young’s modulus, and yield strength. For compression test specimens, these parameters were infill percentage, number of shells, and print orientation angle. For tensile test specimens, the parameters were layer height, number of shells, and infill orientation angle. Pre- and post-compression test samples were evaluated by scanning electron microscopy for microstructural analysis. Infill percentage had the greatest effect on mechanical properties while number of shells and print orientation angle had minor effects. When changing the layer lines from perpendicular to parallel, relative to the loading direction, SiC-PLA had higher mechanical properties while pure PLA properties had decreased, and zirconium silicate-PLA had mix results.

Fused filament fabrication

Tensile Strength and Microstructural Characterization of Uncoated and Coated HPZ Ceramic Fibers

Tensile strengths of as-received HPZ fiber and those surface coated with BN, BN/SiC, and BN/Si3N4 have been determined at room temperature using a two-parameter Weibull distribution. Nominally approx. 0.4 micron BN and 0.2 micron SiC or Si3N4 coatings were deposited on the fibers by chemical vapor deposition using a continuous reactor. The average tensile strength of uncoated HPZ fiber was 2.0 +/- 0.56 GPa (290 +/- 81 ksi) with a Weibull modulus of 4.1. For the BN coated fibers, the average strength and the Weibull modulus increased to 2.39 +/- 0.44 GPa (346 +/- 64 ksi) and 6.5, respectively. The HPZ/BN/SiC fibers showed an average strength of 2.0 +/- 0.32 GPa (290 +/- 47 ksi) and Weibull modulus of 7.3. Average strength of the fibers having a dual BN/Si3N4 surface coating degraded to 1.15 +/- 0.26 GPa (166 +/- 38 ksi) with a Weibull modulus of 5.3. The chemical composition and thickness of the fiber coatings were determined using scanning Auger analysis. Microstructural analysis of the fibers and the coatings was carried out by scanning electron microscopy and transmission electron microscopy. A microporous silica-rich layer approx. 200 nm thick is present on the as-received HPZ fiber surface. The BN coatings on the fibers are amorphous to partly turbostratic and contaminated with carbon and oxygen. Silicon carbide coating was crystalline whereas the silicon nitride coating was amorphous. The silicon carbide and silicon nitride coatings are non-stoichiometric, non-uniform, and granular. Within a fiber tow, the fibers on the outside had thicker and more granular coatings than those on the inside.

Bansal, Narottam P.

Directed energy deposition of Haynes 282 nickel superalloy

Laser powder directed energy deposition was employed to fabricate Haynes® 282 Ni-based superalloy for high temperature creep testing. Material was heat treated using a single-step aging heat treatment of 800 °C for 4 h. Microstructural analysis was conducted in the as-deposited, solution-annealed, and age-hardened conditions. γ′ precipitates were absent in the as-deposited and annealed condition but formed during aging with an average size of 48.5 ± 12 nm. γ’ denuded zones ranging in thickness from 73 to 469 nm were observed adjacent to an effectively continuous grain boundary carbide film that covered 72.5% of the measured boundary length. The heat-treated material contained a high-volume fraction of TiC carbides ranging in size from 38 to 457 nm. Electron backscatter diffraction showed partial recrystallization, with 77-83% recrystallized area and a heterogeneous grain-size distribution. Creep testing at 750 °C at 300, 320, and 350 MPa revealed significantly inferior performance compared to wrought material, with higher strain rates, earlier tertiary onset, and shorter rupture lives. Fractography shows that failure was dominated by intergranular rupture. Post rupture microstructural analysis results suggest that the creep behavior was primarily governed by the non-equilibrium interface network rather than the bulk γ/γ’ matrix. In conclusion, the findings indicate that achieving wrought-like creep performance necessitates substantial improvements in the additive process, specifically focusing on enhanced homogenization, full recrystallization, and precise control over the morphology and distribution of carbides.

36 - MATERIALS SCIENCE

Voltage cycling as a dynamic operation mode for high temperature electrolysis solid oxide cells

Solid Oxide Electrolysis Cells (SOECs) have emerged as a promising technology for the efficient production of H2 via high-temperature electrolysis. However, power input from dynamic energy sources remains a significant challenge for their long-term stability. It is important to analyze the tolerance of cells under dynamic operation conditions. This study focuses on evaluating the impact of voltage cycling on the performance and durability of electrode-supported SOECs. We explore the operational limits and degradation mechanisms of SOECs subjected to various voltage conditions and find that the cells have high tolerance for dynamic voltage. Voltage cycling between 1.3 V and 1.5 V for 9000 cycles does not damage the cell. Conversely, cycling to higher voltages (≥1.7 V) results in accelerated degradation. Advanced characterization is used to screen for various degradation modes post operation. Within the oxygen electrode, XRD and STEM EDS find compositional and phase evolution in all voltage cycled samples including increased decomposition of the air electrode resulting in cation migration. Microstructural analysis of the fuel electrode from nano-CT data shows minimal change throughout the sample set and no evidence of Ni migration, indicating the fuel electrode is stable and not impacted by cycling to higher voltages within the timeframe studied.

Zhu, Zhikuan

Sputter coating of Nb₃Sn into SRF cavity using stoichiometric target

Nb₃Sn has emerged as a leading alternative material due to its higher superconducting critical temperature (Tc) and superheating field (Hsh), promising a viable solution to the intrinsic performance limit currently faced by Nb superconducting radiofrequency (SRF) cavities. We sputter-coated Nb₃Sn inside Nb SRF cavity using a stoichiometric Nb₃Sn tube target in a DC cylindrical magnetron sputter coater. The target was fabricated by growing an estimated >20 μm thick Nb₃Sn layer on a Nb tube via Sn vapor diffusion using Jefferson Lab’s coating system. Approximately 150 nm thick Nb-Sn films were sputter-deposited onto flat Nb samples at positions representing the beam tubes and equator of a 2.6 GHz Nb cavity. Post-deposition annealing at 950 °C for 3 h resulted in the formation of Nb₃Sn. Microstructural analysis of the annealed films was carried out to investigate the morphology and structure of the Nb₃Sn films. Later, a 2.6 GHz Nb SRF cavity was coated with a ~1.2 μm thick sputtered Nb-Sn film using a stoichiometric Nb₃Sn target, followed by annealing. Cryogenic RF testing of the annealed cavity demonstrated a Tc of 17.8 K, indicating the formation of Nb₃Sn. After a light Sn recoating treatment, the cavity achieved a quality factor (Q0) of 6.7E+08 at lower field at 2.0 K.

Accelerator Physics