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At least 37 records · Page 2

Application of the cubic polynomial strength criterion to the failure analysis of composite materials

A comparative failure analysis is presented based on the application of quadratic and cubic forms of the tensor polynomial lamina strength criterion to various composite structural configurations in a plane stress state. Failure loads have been predicted for off-angle laminates under simple loading conditions and for symmetric-balanced laminates subject to varying degrees of biaxial tension, including configurations subject to multimode failures. Some experimental data are also provided to support these calculations. From these results, the necessity of employing a cubic strength criterion to accurately predict the failure of composite laminae is demonstrated.

Tennyson, R. C.

Smaller and faster: a review of conventional and nanocalorimetry techniques for determining thermophysical properties of nuclear materials

Thermal analysis of nuclear materials is critical for the advancement of nuclear technology. The heat effects associated with heat capacity, phase transformation, and radiation damage can be measured with conventional calorimeters. However, conventional calorimetric techniques are often restricted in terms of heating rate and sample mass, especially when studying the limited amounts of materials subject to extreme conditions. In this review, we summarize conventional calorimetric studies of critical thermophysical and thermochemical properties of pure actinide metals (U, Np, Am, Pu), fast reactor metallic fuel alloy systems (U–Zr, U–Pu–Zr, Pu–U, Pu–Zr), and actinide oxides that are primary constituents or transmutation products in light water reactor fuel rods (U–O, Np–O, Am–O, Pu–O, Pu–U–O). Adiabatic and drop calorimetry have been the primary techniques used for these studies, however the development of fast scanning calorimetry using micro-electro-mechanical-based systems allows determination of thermodynamic properties from smaller sample masses. We report recent investigations that leverage the fast heating rates of nanocalorimetry by itself or combined with other characterization techniques. Furthermore, we then discuss opportunities for nanocalorimetry to provide solutions to some of the technical challenges inherent in thermal analysis of nuclear materials, namely a reduction in sample activity, emulating heating transients, investigation of phase evolution in irradiated samples, and characterization of radiation damage evolution. Nanocalorimetry has the potential to significantly advance the understanding of thermophysical properties in nuclear materials and thus accelerate the development of nuclear technology.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS

Material Properties and Modeling of Room Temperature Vulcanizing Silicone

Room Temperature Vulcanizing silicone (RTV) is a high-temperature adhesive that has successfully been used as a gap-filler between Thermal Protection System (TPS) tiles for heatshields on numerous missions. It is also used to bond instrumentation plugs such as temperature and pressure sensors into the heatshields. While RTV has been traditionally assumed to be a non-porous and non-ablating material, numerous experiments have shown that RTV pyrolyzes and becomes highly porous as it is heated. Heating RTV has also shown swelling, or intumescence, which can pose unique problems that lead to roughness induced boundary-layer transition, surface oxide formation and contamination of heat shield sensors. Therefore, it is crucial to understand and model the intumescence phenomenon of RTV. As data for RTV material properties is limited, the first step in modeling RTV is to collect material properties such as pyrolysis mass-loss, microstructure change, virgin and char porosity, etc. which was performed in our initial study. Additionally, thermomechanical properties such as Young’s modulus and Poisson ratio are required for modeling the intumescence of RTV, which were taken from literature and the coefficient of thermal expansion was collected using in-situ heating and Micro Computed Tomography (µ-CT) in previous studies. Finally, numerous other properties such as pyrolysis gas properties, virgin and char thermal conductivity and specific heat were compiled from previous experiments and literature into a material database that can be used for simulations. In Porous Material Analysis Toolbox based on OpenFOAM (PATO) [4], structural mechanics coupled with material response was used for simulating the intumescence of RTV as it is heated. However, since the permeability of the material is very low, the pyrolysis gas creates an internal pressure build-up as the material is being heated, significantly contributing to the deformation of the material. To correctly characterize this phenomenon, additional physics models were implemented into PATO's stress analysis solver, and results were compared with RTV dilatometry test data as a preliminary verification case. Future work will include experiments of RTV at the Plasmatron X facility and the in-situ heating cell with µ-CT, and improvement of simulation tools to more accurately model RTV intumescence.

PATO

Patch-Based Convolutional Neural Networks for Multiple Microstructural Features Detection in FIB-SEM Micrographs of Irradiated Nuclear Fuel

Focused ion beam scanning electron microscopy (FIB-SEM) tomography has increasingly been utilized for acquiring three-dimensional (3D) microstructure features at the sub-micron scale in irradiated nuclear materials. This technique involves sequential ion beam slicing followed by electron beam imaging and compositional mapping using energy dispersive spectroscopy (EDS). Despite its growing use, several challenges persist. These include the time-intensive nature of data collection of EDS data, difficulties in distinguishing between various microstructures, and issues with image alignment. These challenges currently limit the broader application of FIB-SEM tomography in the field. To overcome these limitations, we propose using convolutional neural networks (CNNs) to automate microstructure identification in SEM images. Our study introduces a new framework for identifying microstructures in irradiated U-10Zr (wt. %) metallic fuel with limited annotated data. The framework includes the creation of a reliable annotated dataset with paired SEM and ground truth data from EDS maps, the applications of CNNs for microstructure identification, and the validation of model performance. Specifically, we employed the Segment Anything Model (SAM) to align SEM images with corresponding EDS maps and focused ion beam (FIB) tomography SEM data. We evaluate several models, including Patch-based U-Net, Attention U-Net, and Residual U-Net, finding that patch-based U-Net exhibits superior segmentation performance and consistency. This approach reduces reliance on EDS detectors and aids in accelerating nuclear material analysis process, highlighting the potential of advanced deep learning techniques to improve microstructural understanding in nuclear material. This is the first framework to integrate SAM and Patch-based CNN models for semantic segmentation of irradiated nuclear materials, with potential applicability to other tomography datasets.

36 - MATERIALS SCIENCE

Coal gasification systems engineering and analysis. Appendix A: Coal gasification catalog

The scope of work in preparing the Coal Gasification Data Catalog included the following subtasks: (1) candidate system subsystem definition, (2) raw materials analysis, (3) market analysis for by-products, (4) alternate products analysis, (5) preliminary integrated facility requirements. Definition of candidate systems/subsystems includes the identity of and alternates for each process unit, raw material requirements, and the cost and design drivers for each process design.

Source record

Design, durability and low cost processing technology for composite fan exit guide vanes

A lightweight composite fan exit guide vane for high bypass ratio gas turbine engine application was investigated. Eight candidate material/design combinations were evaluated by NASTRAN finite element analyses. A total of four combinations were selected for further analytical evaluation, part fabrication by two ventors, and fatigue test in dry and wet condition. A core and shell vane design was chosen in which the unidirectional graphite core fiber was the same for all candidates. The shell material, fiber orientation, and ply configuration were varied. Material tests were performed on raw material and composite specimens to establish specification requirements. Pre-test and post-test microstructural examination and nondestructive analyses were conducted to determine the effect of material variations on fatigue durability and failure mode. Relevant data were acquired with respect to design analysis, materials properties, inspection standards, improved durability, weight benefits, and part price of the composite fan exit guide vane.

Blecherman, S. S.

Measuring Loss Tangents of Substrates for Superconducting Qubits with Part-per-Billion Precision

We report precision measurements of dielectric loss tangents in substrates for superconducting qubits using an ultra-high quality factor niobium SRF cavity operating at millikelvin temperatures and low electric fields. Multiple substrate types and surface treatments are compared to assess how processing impacts microwave dissipation. The RF results are correlated with materials analysis, including ToF-SIMS and XPS, to identify dominant loss mechanisms. This combined study links microscopic surface chemistry to macroscopic performance and provides a framework for materials-driven improvements in qubit coherence and device design.

Bafia, Daniel [Fermilab]

Measuring Loss Tangents of Substrates for Superconducting Qubits with Part-per-Billion Precision

We report precision measurements of dielectric loss tangents in substrates for superconducting qubits using an ultra-high quality factor niobium SRF cavity operating at millikelvin temperatures and low electric fields. Multiple substrate types and surface treatments are compared to assess how processing impacts microwave dissipation. The RF results are correlated with materials analysis, including ToF-SIMS and XPS, to identify dominant loss mechanisms. This combined study links microscopic surface chemistry to macroscopic performance and provides a framework for materials-driven improvements in qubit coherence and device design.

Bafia, Daniel [Fermilab]

Single-Particle Isotopic Analysis Using the Liquid Sampling-Atmospheric Pressure Glow Discharge Microplasma Coupled to an Orbitrap Mass Spectrometer

Isotope ratio (IR) determinations on individual particles can provide valuable information relative to the sample, including processing and dating, which could be valuable to geological and nuclear material analysis communities. In comparison to “bulk” measurements, in which all particle information is lost and homogenized within a sample, “particle” measurements allow for fingerprinting and can provide unique insights related to the sample’s nano- and micro- compositions. Furthermore, the complex nature of particles, with potential isobaric interferences from either the matrix or other elements within the same particle, poses a significant analytical challenge for conventional mass spectrometry platforms employed for elemental analysis due to their limited mass resolution. Presented here is the first demonstration of an ultrahigh resolution method for single particle (SP) isotopic analysis using the liquid sampling-atmospheric pressure glow discharge (LS-APGD) microplasma ionization source coupled to an Orbitrap mass spectrometer and FTMS Booster X2T acquisition/processing system. For proof of concept, well-characterized CeO 2 microparticles with a nominal diameter of 1.0 μm were analyzed at a mass resolution of ∼330,000. Important instrumental parameters were optimized to enable the detection of single particles. The 142 Ce/ 140 Ce ratio of individual particles and the population average were determined and compared to an SP inductively coupled plasma time-of-flight mass spectrometry (ICP-TOF-MS) analysis. The isotopic accuracy and precision were determined by two methods and found to be in good agreement with the SP-ICP-TOF-MS method, with the linear regression slope method providing a more accurate ratio, showing a ∼1.4% relative difference from the ratio determined from a particle digest. The encouraging performance of the method was further supported by a determined detection limit of 2.9 fg ( 142 Ce). The developed method is anticipated to overcome many of the challenges posed by isobaric interferences encountered in conventional mass spectrometry techniques when analyzing real-world samples for particle isotopic composition.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH

Characterizing microscale signatures in uranium ore concentrates using electron probe microanalyzer

Impurities in uranium ore concentrates (UOCs) serve as forensic signatures of processing history and origin. Here, this study utilizes Electron Probe Microanalyzer (EPMA) to characterize microscale compositional and textural features in individual UOC particles from both commercial and bench-scale production. At the particle scale, multiple internal phases with distinct morphologies, chemical signatures, and stoichiometries are documented. Our data shows that chemical impurities are heterogeneously distributed within single particles and among particles within a sample. These microscale heterogeneities correlate with known processing histories, indicating that microscale signatures of early fuel cycle materials can provide valuable information for nuclear forensic material analysis.

organic

Thermo-Poro-Mechanical Modeling of RTV Intumescence

Room temperature vulcanizing (RTV) silicone is a high-temperature adhesive used as a gap-filler between heatshield tiles in numerous entry missions. Its propensity to intumesce, or swell upon exposure to heat, is a well-known effect that needs to be carefully quantified during design. At tile interfaces of charring ablators, intumescence, combined with differential recession, could cause the gap filler to protrude past the ablator outer mold line, forming a “fence”. Fencing can in turn cause transition to turbulence of the flow wetting the heat shield, leading to augmented surface heating. Recent experiments conducted at the Plasmatron X facility, the high enthalpy wind tunnel of the Center for Hypersonics and Entry Systems Studies, have shown prominent fencing of RTV gap fillers in PICA, under both nitrogen and air plasmas. Similar observations are well known in the arcjet literature. Further experiments under controlled environment, performed using in situ X-ray micro-computed tomography (micro-CT) at the Advanced Light Source (ALS), have shown heating rate-dependent swelling and shrinkage of RTV during pyrolysis. To simulate RTV intumescence, a novel model was introduced in the Porous Materials Analysis Toolbox based on OpenFOAM, PATO, to account for pore-pressure buildup within both closed- and open-pores. The governing equation for the thermo-poro-mechanical response were developed, assuming linear elasticity for the charring silicone. A new multi-pyrolysis model that tracks non-monotonic advancement of material properties with pyrolysis was proposed. This model addresses the limitations of state-of-the-art ablator models to capture the different stages of thermal degradation and coupled thermomechanics. Swelling of RTV was simulated using the new thermo-poro-mechanical model and compared against in situ micro-CT data. Results showed good agreement in intumescence height and temperature profiles at all heating rates, indicating that the key factor contributing to RTV swelling is the internal pressure build-up within closed- and open-pores. As RTV is cured into a soft (rubbery) compound with low-porosity and permeability, initial temperature increase and pyrolysis gas production cause a significant increase of internal pressure, causing a pronounced volume growth. As thermal degradation progresses, rigidization of the silicone occurs due to char hardening which counteract volume shrinkage after gas pressure relief. Overall, our model shows that accounting for changes in properties such porosity, permeability and key thermomechanical coefficients is crucial for capturing the RTV volume change during ablation and enable a predictive capability for heatshield tile interface response. A plan for future calibration of thermomechanical properties evolution during degradation is discussed, as a key next step to close the new model.

RTV

Thermo-Poro-Mechanical Modeling of RTV Intumescence

Room temperature vulcanizing (RTV) silicone is a high-temperature adhesive used as a gap-filler between heatshield tiles in numerous entry missions. Its propensity to intumesce, or swell upon exposure to heat, is a well-known effect that needs to be carefully quantified during design. At tile interfaces of charring ablators, intumescence, combined with differential recession, could cause the gap filler to protrude past the ablator outer mold line, forming a “fence”. Fencing can in turn cause transition to turbulence of the flow wetting the heat shield, leading to augmented surface heating. Recent experiments conducted at the Plasmatron X facility, the high enthalpy wind tunnel of the Center for Hypersonics and Entry Systems Studies, have shown prominent fencing of RTV gap fillers in PICA, under both nitrogen and air plasmas. Similar observations are well known in the arcjet literature. Further experiments under controlled environment, performed using in situ X-ray micro-computed tomography (micro-CT) at the Advanced Light Source (ALS), have shown heating rate-dependent swelling and shrinkage of RTV during pyrolysis. To simulate RTV intumescence, a novel model was introduced in the Porous Materials Analysis Toolbox based on OpenFOAM, PATO, to account for pore-pressure buildup within both closed- and open-pores. The governing equation for the thermo-poro-mechanical response were developed, assuming linear elasticity for the charring silicone. A new multi-pyrolysis model that tracks non-monotonic advancement of material properties with pyrolysis was proposed. This model addresses the limitations of state-of-the-art ablator models to capture the different stages of thermal degradation and coupled thermomechanics. Swelling of RTV was simulated using the new thermo-poro-mechanical model and compared against in situ micro-CT data. Results showed good agreement in intumescence height and temperature profiles at all heating rates, indicating that the key factor contributing to RTV swelling is the internal pressure build-up within closed- and open-pores. As RTV is cured into a soft (rubbery) compound with low-porosity and permeability, initial temperature increase and pyrolysis gas production cause a significant increase of internal pressure, causing a pronounced volume growth. As thermal degradation progresses, rigidization of the silicone occurs due to char hardening which counteract volume shrinkage after gas pressure relief. Overall, our model shows that accounting for changes in properties such porosity, permeability and key thermomechanical coefficients is crucial for capturing the RTV volume change during ablation and enable a predictive capability for heatshield tile interface response. A plan for future calibration of thermomechanical properties evolution during degradation is discussed, as a key next step to close the new model.

silicone intumescence