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At least 127 records · Page 7

Improving protonic ceramic electrochemical cell performance via a dual-phase reaction-sintered bilayer electrolyte

Protonic ceramic electrochemical cells (PCCs) are promising energy conversion devices, but their fabrication remains challenging. In particular, the typical electrolytes for PCCs such as BaCe 0.7 Zr 0.1 Y 0.1 Yb 0.1 O 3−δ (7111) and BaCe 0.4 Zr 0.4 Y 0.1 Yb 0.1 O 3−δ (4411) suffer from intrinsic barium evaporation issues during high-temperature sintering. This tendency towards barium loss, combined with their highly refractory nature, leads to a tradeoff between sinterability and chemical stability. To address this tradeoff, we propose a bilayer electrolyte combining layers of 4411 and 7111 materials that is designed to enhance sinterability and conductivity through dual-phase reactive sintering. Our findings demonstrate that the bilayer structure exhibits shrinkage behavior closely matched to that of the fuel electrode substrate, with a higher shrinkage compared to a single-layer 4411 electrolyte. Utilizing this bilayer electrolyte structure, our PCCs achieve a peak power density of 637 mW∙cm −2 in fuel-cell mode and a current density of 1060 mA∙cm −2 at 1.3 V in electrolysis mode at 600 °C. Our PCCs demonstrate high Faradaic efficiency of 83% at 1.3 V and 500 °C. Hybrid distribution of relaxation times (DRT) polarization mapping further reveals that the bilayer structure reduces Ohmic and polarization resistance in both fuel-cell and electrolysis modes.

ceramic processing↗

Effect of calcite filler on carbonation behavior in a synthesized C‐S‐H binder

Widespread implementation of portland limestone cements (PLC) in industry has raised new questions about their carbonation resistance due to higher initial limestone content than ordinary portland cement. While carbonation of portland cement and each of its hydrate phases has been studied at a fundamental level, the integral role of how limestone fillers interact chemically or physically during carbonation necessitates further study. In this study, a C-S-H binder comprised of a highly reactive zeolite pozzolan and lime was used to evaluate the effect of varying calcite additions on carbonation behavior at a microstructural level. Fundamental insight into hydration kinetics and carbonation mechanisms of hydraulic binders was obtained via analysis of the C-S-H and calcite microstructure. X-ray microcomputed tomography (X-ray CT) was used to quantify microstructural changes, and the results showed a decrease in shrinkage for increased calcite dosages, with a ∼50% reduction observed for a 45% wt. calcite replacement level. Crystallographic and thermal analyses measured compositional changes in the binder and confirmed that shrinkage was related to the decalcification of C-S-H. Furthermore, the addition of calcite to the C-S-H binder effectively reduced the liquid-to-solid ratio, porosity, and amount of C-S-H present in these binders. Ultimately, these results help elucidate how the carbonation risks of PLC can be mitigated by proportioning the mixture water only to the reactive component of the binder.

C-S-H↗

Microstructure Experiments-Enabled MARMOT Simulations of SiC/SiC-based Accident Tolerant Nuclear Fuel System

We have undertaken an experimental-computational project that addresses a few key technology gaps associated with the use of SiC/SiC composites for light water reactor fuel cladding. Two principal endeavors in this project are to assess the irradiation-induced microstructural changes and swelling in SiC/SiC composites, and to characterize and model the porous oxide surface layer (when exposed to steam) along SiC recession that is detrimental to the clad integrity under accident conditions. The project tasks are: (i) ion irradiation and characterization (University of Tennessee, Knoxville), (ii) mechanical tests and analysis (University of South Carolina), (iii) steam exposure tests (Oak Ridge National Laboratory), (iv) electron microscopy and spectroscopic characterization (NC State University), (v) x-ray microscopy and reconstruction (University of South Carolina and NC State University), (vi) phase field modeling and simulations (NC State University and Idaho National Laboratory). The effects of 10 MeV Au ion irradiation at 350°C on the microstructure evolution in SiC/SiC composites are investigated at doses up to 400 displacements per atom (dpa) at the University of Tennessee, Knoxville. Atomic force microscopy and optical profilometry reveal irradiation induced axial and radial shrinkage of the fibers for doses greater than 10 dpa. Based on detailed electron microscopy characterization, the primary cause of the fiber shrinkage is attributed to irradiation-induced loss of carbon packets. Additionally, the multilayer PyC interface is observed to portray high resistance to irradiation damage. The mechanical response and failure mechanisms of un-irradiated samples is also assessed through loading tests and X-ray imaging at the University of South Carolina. Steam exposure tests are performed at the Oak Ridge National Laboratory in a facility that represents a reactor pressure vessel under a loss-of-coolant-accident scenario. The samples that are analyzed methodically in this report are tested for 32/31 hours at 1200°C with a velocity of 0.25 cm/s for the pressures: 0.1 MPa, 0.45 MPa, 0.92 MPa and 1.38 MPa. Scanning/transmission electron microscopy analysis conducted at the NC State University (NCSU) shows that the oxide layer thickness increases with the steam pressure. While the oxide layer is crystalline (α- cristobalite) for the pressures 0.45 MPa, 0.92 MPa and 1.38 MPa, the layer is amorphous at 0.1 MPa. Results from Raman spectroscopy have also confirmed the formation of α-cristobalite phase of SiO₂. The abrupt increase in the integrated Raman intensity ratio between steam pressures 0.1 and 0.45 MPa suggests the onset of accelerated crystallization. Non-destructive three dimensional X-ray microscopy/tomography (XCT) and computational image processing techniques are employed by the University of South Carolina to probe the porous oxidation features on SiC samples at varying pressures. Interestingly, most pores are observed to be located away from the surface as well as the oxide-SiC interface. The average oxide layer thickness assessed from the XCT analysis is seen to be in excellent agreement with the values determined through scanning electron microscopy analysis for the highest pressures where the oxide layer is relatively more uniform. A phase-field model developed by the NC State University and Idaho National Laboratory for simulating oxidation of SiC by steam captures the paralinear kinetics of SiC oxidation with a high degree of fidelity. Results from quasi-one-dimensional and two dimensional simulations show that the pores with oxidizing species lead to a higher volatilization rate. These simulations indicate that the enhanced apparent volatilization rates at higher pressures observed in experiments can be rationalized by the increased volatilization from the pores. The project team has also successfully developed the capability to import images from experiments for realistic evolution of the oxidizing microstructure.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Dynamic Behavior of Natural Seep Vents: Analysis of Field and Laboratory Observations and Modeling (Final Scientific/Technical Report)

In this project, we have analyzed data collected by the U.S. Department of Energy (DOE), National Energy Technology Laboratory (NETL) in a high pressure water tunnel (HPWT) and data from two research cruises to natural seeps in the Gulf of Mexico to adapt and validate a numerical model to predict the dynamics of natural seeps in the deep oceans. The HPWT data include video observations of the shrinkage rate of individual methane and natural gas bubbles under simulated deep-water conditions. Field data were collected during two cruises by the Gulf Integrated Spill Research (GISR) Consortium led by Texas A&M University and funded by the Gulf of Mexico Research Initiative (GoMRI). These data included in situ observations from a remotely operated vehicle (ROV) of gas bubbles at two natural seep sites in the Gulf and acoustic observations of the natural seep bubble flares in the ocean water column. The acoustic data were from multibeam echosounders, one mounted in a forward-looking orientation on the ROV and another mounted down-looking in the haul of the ship. All of these laboratory and field data were focused on the dynamics of natural gas bubbles at temperatures and pressures favorable for clathrate hydrate formation between the gas and water. Our analyses of this data focused on understanding the mechanisms responsible for gas bubble dissolution within the hydrate stability zone (HSZ) of the oceans. Ice-like hydrate shells may form on the bubble-water interface under these conditions, and it was unknown how this might affect the mass transfer of gas into the ocean. We were able to extract bubble shrinkage rates from the HPWT datasets. Using this data we determined that mass transfer coefficients with and without a hydrate shell match empirical values for bubbles in contaminated systems (so-called dirty bubbles contaminated by naturally occurring surfactants). We also showed that free gas, and not gas hydrate, is the dominant dissolving phase when the hydrate sub-cooling is below 11 degree Celsius (temperature difference between hydrate the hydrate formation temperature and ambient temperator) or the pressure is reducing as bubbles rise through the ocean water column. Using this mass transfer model, our numerical model of bubble dissolution matched the over 200 HPWT experiments with an average error of 10% for predicting the bubble size at the end of an experiment. From field data in the literature, we also observed that gas bubbles dissolve faster when they are initially released, following mass transfer coefficients for so-called clean-bubbles (those not yet contaminated by surfactants). Shortly after release within the HSZ, a hydrate shell forms on the bubble-water interface, and the mass transfer reduces to rates matching those of dirty bubbles. We correlated this transition time from clean to dirty bubble behavior with the initial bubble surface area and the hydrate sub-cooling. With this model for hydrate formation time and using the mass transfer coefficients deduced from the HPWT data, we validated our numerical model for predicting the rise heights of natural seep flares in the oceans. Flare heights are commonly observed in haul-mounted acoustic multibeam data. The numerical model predicts bubbles to rise high in the ocean water column owing to the slower mass transfer rates for dirty bubbles that accompany the majority of their rise time. We found that the numerical model predictions matched the observed flare heights within 5% to 10% accuracy when we compared the rise heights of the largest bubbles released from the seafloor with the bubbles acoustically visible in the multibeam data. Bubbles become acoustically transparent as they shrink to sizes of order 1 mm in diameter for the multibeam frequencies used in the field. The forward-looking multibeam on the ROV also provided data on the lateral spreading of bubbles in natural seep flares. Our analysis of this data showed that spreading follows a diffusion process, with the effective diffusivity correlating with the wobbling length scale of these ellipsoidal bubbles. When we apply this diffusivity in a random displacement model of bubble spreading, our numerical simulations match closely the lateral spread observed by the M3 in the ocean water column. Finally, we compared the seep model predictions for the acoustic properties of these natural seep plumes with that observed by the acoustic instruments in the field. The M3 and EM 302 observations were converted to relative values of target strength using a calibration we obtained in the laboratory for the M3 and using an algorithm from the manufacturer for the EM 302. Comparing the numerical seep model to these data, we obtain good agreement over the whole height of rise of these bubble flares. This further validates the numerical model. Overall, our validated seep model captures the key dynamics of gas bubbles released from natural seeps in the oceans and helps to predict the fate of methane in the water column.

03 NATURAL GAS↗

Integrated Multiphysics Modeling of Environmentally Assisted Brittle Fracture

Brittle materials, such as cement, compose major portions of built infrastructure and are vulnerable to degradation and fracture from chemo-mechanical effects. Currently, methods of modeling infrastructure do not account for the presence of a reactive environment, such as water, on the acceleration of failure. Here, we have developed methodologies and models of concrete and cement fracture that account for varying material properties, such as strength, shrinkage, and fracture toughness due to degradation or hydration. The models have been incorporated into peridynamics, non-local continuum mechanics methodology, that can model intersecting and branching brittle fracture that occurs in multicomponent brittle materials, such as concrete. Through development of new peridynamic capabilities, decalcification of cement and differential shrinkage in clay-cement composites have been evaluated, along with exemplar problems in nuclear waste cannisters and wellbores. We have developed methods to simulate multiphase phenomena in cement and cement-composite materials for energy and infrastructure applications.

36 MATERIALS SCIENCE↗

Convergent Manufacturing of Large-Scale Components for Nuclear Applications, via Additive Manufacturing and Powder Metallurgy Hot Isostatic Pressing

Powder metallurgy (PM)–hot isostatic pressing (PM-HIP) has long been recognized as a powerful route for producing fully dense, near net shape metallic components. By consolidating powders under high temperature and pressure, HIP provides isotropic properties, uniform microstructures, and scalability to complex geometries that are vital for sectors such as aerospace, energy, and nuclear power. Yet despite these advantages, the technology has remained constrained by costly trial and error canister fabrication, limitations of conventional forging, and incomplete knowledge about how the canister design influences final part properties. Additive manufacturing (AM), by contrast, thrives on design freedom and geometric flexibility but struggles with speed, scalability, and cost when applied to very large structures. The research presented in this report investigated how a convergent manufacturing approach, combining AM with PM-HIP, can merge the strengths of both technologies, leveraging AM’s flexibility for canister design and HIP’s consolidation capability to deliver reliable, large, and complex parts. The work progressed through three case studies that built on one another in scale and complexity. Small cylindrical canisters fabricated by conventional methods, laser powder bed fusion, and directed energy deposition were filled with stainless steel powders and subjected to HIP. The resulting parts demonstrated near-full density and mechanical properties on par with wrought stainless steel, showing for the first time that AM canisters can be a direct substitute for conventional ones without sacrificing quality. The next step involved a medium-scale, noncentrosymmetric T-valve, which is an enclosed, multibranch geometry that tested the limits of AM + PM-HIP integration. The T-valve achieved predictable shrinkage and uniform densification, confirming feasibility for enclosed designs. However, this study also revealed oxide inclusions and interfacial challenges at the AM + HIP boundary, underscoring the critical importance of controlling interface chemistry and employing robust, in situ strategies, such as melt pool monitoring and thermal monitoring, coupled with nondestructive evaluation techniques such as x-ray computed tomography. Finally, the effort culminated in fabricating a large-scale impeller weighing nearly 2000 lb and spanning 5 ft in diameter. Produced via multirobot wire arc AM and hot isostatic pressed to near-full density, the impeller validated industrial-scale feasibility. Predictive models closely matched experimental shrinkage, tensile properties were spatially uniform across the component, and the AM + PM-HIP interface proved mechanically sound despite the presence of oxide-decorated prior particle boundaries. This large-scale demonstration is a major milestone, showing that hybrid AM + PM‑HIP can reliably deliver components at reactor-relevant scales. Collectively, these studies charted a logical pathway: small-scale work built scientific confidence, medium-scale work highlighted opportunities and challenges, and large-scale work proved industrial impact. The overarching conclusion of this report is that AM + PM-HIP should not be seen as a replacement for forging but as a complementary pathway that provides the US with flexibility, resilience, and new options for manufacturing nuclear-grade components. Looking ahead, several directions emerge as critical to sustaining progress. Predictive modeling must become faster, more accessible, and more accurate, with digital twins and machine learning reducing reliance on trial and error. Powders and alloys must be optimized for HIP, with improved cleanliness, reduced oxides, and tailored chemistries that enhance creep, fatigue, and irradiation resistance. Interfaces between AM and HIP regions must be better engineered through coatings, machining strategies, and surface treatments to mitigate oxide formation and ensure reliable bonding to explore opportunities for HIP of targeted compositional parts, as well as multimaterial HIP cladding applications. Monitoring and nondestructive evaluation need to expand, incorporating multimodal sensors, x-ray computed tomography, and real-time data integration through platforms such as Pelican. At the same time, the pathway to industrial adoption requires techno-economic analysis, machinability studies, and qualification frameworks aligned with industry and regulatory standards. Finally, workforce and academic engagement must be strengthened. Programs that train technicians and engineers for US Navy and US Department of Energy manufacturing challenges should be paired with academic partnerships to support fundamental research, with open sharing of non-export-controlled data to accelerate innovation and build the next generation of experts. In conclusion, this report demonstrates that hybrid AM + PM-HIP is scientifically viable and strategically important. By combining the design agility of AM with the consolidation strength of HIP and embedding modeling, monitoring, and workforce development, this approach provided a transformative new capability for US manufacturing. The path forward is clear: hybrid AM + PM-HIP is not just a promising research direction but is also potentially an industrially relevant pathway that can reshape how nuclear-grade components are designed, qualified, and deployed.

36 MATERIALS SCIENCE↗

Contact material for pressure-sintering ferrites

Pressure-sintering, in which the unfired laminated ferrite plane is placed between two flat punches and pressed during firing, reduces lateral firing shrinkage to less than one percent. A decrease in thickness of the laminate produces the required volume shrinkage. Phlogopite is the most suitable contact material investigated.

Wentworth, C.↗

Circuit breaker cases

A flammable plastic part was duplicated dimensionally using a nonflammable material in place of the flammable plastic. The material used was L-3203-6 with a 16-hour post-cure at 400 F. Initial efforts were made to determine shrinkage tolerances required to produce a mold which would produce a finished, workable part. The final twenty-five circuit breaker cases were shipped and the metal inserts when installed, produced a workable breaker. Initial submissions of cases were rejected as lacking sufficient rigidity though they met all other requirements. The plastic cases weighed 16.5 grams, whereas the Refset cases weighed 17 grams, not meeting the less-weight requirement. The data on shrinkage determinations, and mold and part dimensions are shown. The method of manufacture is also reported.

Holmes, R. L.↗

Silica Reusable Surface Insulation Improvement Research

Fiber characterization, fabrication processes, physical properties, and thermal responses are investigated to improve silica reusable surface insulation tiles. Criteria for fiber selection on the basis of chemical composition, shrinkage, and devitrification have been defined and a simple process for fabricating silica surface insulation materials has been developed that produces only 5% shrinkage and no devitrification of tiles at 1533 K in ten hours. Anisotropic tile with improved weak direction strength has been fabricated using conventional molding techniques.

Goldstein, H. E.↗

Carbon microsphere-filled Pyrrone foams.

Syntactic foam formulations were prepared from mixtures of Pyrrone prepolymers and hollow carbon microspheres. Very low curing shrinkages were obtained for high volume loadings of microspheres. The resulting syntactic foams were found to be remarkably stable over a wide range in temperature. A technique was developed for the emplacement of these foam formulations in polyimide-fiberglass, titanium alloy and stainless steel honeycomb without sacrificing low curing shrinkage or thermal stability.

Kimmel, B. G.↗

On possible interactions between upper and lower atmosphere

Geomagnetic data was compared with data on tropospheric and stratospheric circulation characteristics; a statistically significant shrinking was found in areal extent of the stratospheric vortex from the third to the eighth day following a 'geomagnetic storm' The meridionality of the 30 640-m contour line at 10 millibars increases markedly from 5 to 8 days after the storm. During the contraction of the polar vortex edge, the mean height of the vortex central contour decreases only slightly. This indicates that a stratospheric warming event is associated with a steepening of the contour gradient rather than a warming over the entire area of the stratospheric polar vortex. The troposphere reacts to these weak, but significant, stratospheric warming events by a shrinkage of the area of the 500-millibar cold air pool. This shrinkage commences about 3 days after the stratospheric warming. The investigation indicates that the energy input into the stratosphere that is received in conjunction with the geomagnetic disturbance has to come at a propitious time, when the stratospheric-tropospheric circulation system is not already undergoing a major readjustment because of an inherent dynamic instability.

Macdonald, B. C.↗

Weld peaking on heavy aluminum structures

Weld peaking is usually undesirable in any welded structure. In heavy structures, the forces involved in the welding process become very large and difficult to handle. With the shuttle's solid rocket booster, the weld peaking resulted in two major problems: (1) reduced mechanical properties across the weld joint, and (2) fit-up difficulties in subsequent assembly operation. Peaking from the weld shrinkage forces can be fairly well predicted in simple structures; however, in welding complicated assemblies, the amount of peaking is unpredictable because of unknown stresses from machining and forming, stresses induced by the fixturing, and stresses from welds in other parts of the assembly. When excessive peaking is encountered, it can be corrected using the shrinkage forces resulting from the welding process. Application of these forces is discussed in this report.

Bayless, E.↗

Evaluation of low cost/high temperature fiber and blanket insulation

Twelve fiber materials comprising water-felted fiber cakes and blanket insulation were subjected to furnace exposures at 1000, 1200, 1400, and 1600 C for up to 500 hours to establish the time-temperature limits below which these insulation materials can withstand repeated thermal cycles without detrimental shrinkage, thermal conductivity increase, or physical changes. Test samples were inspected periodically during the exposure cycles and weight loss and dimensional shrinkage were measured. Density, fiber crystallography, and thermal conductivity were measured after exposure and properties were compared with those of unexposed controls.

Strauss, E. L.↗

JT9D-70/59 Improved High Pressure Turbine Active Clearance Control System

The JT9D-70/59 high pressure turbine active clearance control system was modified to provide reduction of blade tip clearance when the system is activated during cruise operation. The modification increased the flow capacity and air impingement effectiveness of the cooling air manifold to augment turbine case shrinkage capability, and increased responsiveness of the airseal clearance to case shrinkage. The simulated altitude engine testing indicated a significant improvement in specific fuel consumption with the modified system. A 1000 cycle engine endurance test showed no unusual wear or performance deterioration effects on the engine or the clearance control system. Rig tests indicated that the air impingement and seal support configurations used in the engine tests are near optimum.

Gaffin, W. O.↗

Containerless undercooling and solidification in drop tubes

A containerless low-gravity environment, produced within a 32 m drop tube apparatus, has been used to undercool and solidify metals, alloys or glasses by eliminating crucible induced nucleation processes. Niobium droplets with diameters in the range of 2 to 5 mm have been undercooled by 525 K which corresponds to the maximum undercooling reported by Turnbull and others on fine dispersions of low melting point metals. Solidification at large undercooling resulted in single crystalline spheres with the formation of interdendritic shrinkage channels on the sample surface rather than interior shrinkage cavities. The grain refinement as observed for Ni samples undercooled and solidified in fused silica crucibles does not occur in free-falling drops of Nb. A calculated solidification speed of undercooled Nb is compared to Ni. A solidification speed of 320 m/s is found for the Nb drops. This solidification speed is greater than or comparable to the solidification speeds calculated in splat cooled samples. Thus, a drop tube apparatus can be useful in the preparation and study of high temperature metastable compounds or alloys in bulk form.

Lacy, L. L.↗

The movement of particles in liquid metals under gravity forces and the interaction of particles with advancing solid-liquid interface

The problems of shrinkage and gas porosity are discussed. Gravity forces enhance the removal of gas bubbles from a metal melt and contribute to the feeding of shrinkage porosity in castings. Experiments are reviewed which determine how large a density difference is required for metal particles to float or sink in a metal melt and to what extent do factors not considered in Stokes Law influence particle movement in a real system. As to the interaction of particles with an advancing solid-liquid interface, the results indicate that the metal particles are not rejected in a metal melt, and that concentrations of particles in a metal following solidification are due to other factors.

Weinberg, F.↗

Heavy doping effects in high efficiency silicon solar cells

A model for bandgap shrinkage in semiconductors is developed and applied to silicon. A survey of earlier experiments, and of new ones, give an agreement between the model and experiments on n- and p-type silicon which is good as far as transport measurements in the 300 K range. The discrepancies between theory and experiment are no worse than the discrepancies between the experimental results of various authors. It also gives a good account of recent, optical determinations of band gap shrinkage at 5 K.

Lindholm, F. A.↗

Dendritic growth of undercooled nickel-tin. III

The paper is concerned with structures and microsegregations in undercooled droplets of Ni-25 wt pct Sn and eutectic Ni-32.5 wt pct Sn alloys. An analysis of experimental results suggests that all samples solidify dendritically and that the final structures are largely the result of ripening. Experimental data on minimum solute composition in the samples produced are bounded by two curves both of which assume equilibrium at all liquid-solid interfaces during recalescence and subsequent cooling. The eutectic alloy samples often show a dendritic structure over the surface in areas where shrinkage is present. This structure appears to be the remnant of an original growth structure in which only limited ripening occurred, due to the rapid removal of interdendritic liquid by shrinkage.

Wu, Y.↗