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Ag Nanoparticles Supported on Yttria-Stabilized Zirconia: A Synergistic System within Redox Environments
In this paper, we report a distinctive dynamic sintering-free redox behavior of Ag nanoparticles (AgNPs) on 30 nm thick yttria-stabilized zirconia (YSZ) films. The material system demonstrates reversible 200 nm shifts in the plasmonic spectra with an unprecedented particle phase/size/morphology oscillation during cyclic redox reactions in air and hydrogen/air at 300–400 °C. This is in significant contrast to the minor changes more commonly observed for AgNPs on quartz. It was found that the ionically active YSZ has a strong tendency to drive AgNPs to oxidize under oxidizing conditions, and upon surface oxidation a large differential surface energy is built up, forcing the core/shell particles to migrate and coalesce toward a lower system free energy. Most strikingly, once switched to a mixture of H 2 and air, the previously formed large dewetted metal-core/thick oxide-shell particles collapse, and new small Ag nanoparticles quickly form and remain in a highly dispersed and sintering-free state on YSZ. This is found to likely be due to catalytic production of water over the material system, which plays a key role in the dynamic redox activities. It is hypothesized that the small metallic particle regeneration and sinter-free behavior take place through a four-step process resulting from the synergistic behavior of AgNPs supported on YSZ within a redox environment: (I) production of a local humid environment via catalytic reactions of H 2 and O 2 mostly at the triple-phase boundary, (II) dissolution of Ag + from both reduced Ag and the AgO x shell, (III) collapse and spillover of the AgO x shell/water layer with Ag ions onto the hydrous YSZ surface, and (IV) reduction, diffusion, nucleation, and growth to new small metallic AgNPs with a dynamic equilibrium quickly reached. As a result, the findings behind this novel system could set up an avenue for a new concept of catalysts operating in a self-controlled dynamic regime for governing chemical reactions via metal and ceramic synergized catalysis with high activities and stabilities.
Mycosynthesis of Zinc Oxide Nanoparticles Exhibits Fungal Species Dependent Morphological Preference
Filamentous fungi can synthesize a variety of nanoparticles (NPs), a process referred to as mycosynthesis that requires little energy input, do not require the use of harsh chemicals, occurs at near neutral pH, and do not produce toxic byproducts. While NP synthesis involves reactions between metal ions and exudates produced by the fungi, the chemical and biochemical parameters underlying this process remain poorly understood. Here, the role of fungal species and precursor salt on the mycosynthesis of zinc oxide (ZnO) NPs is investigated. This data demonstrates that all five fungal species tested are able to produce ZnO structures that can be morphologically classified into i) well-defined NPs, ii) coalesced/dissolving NPs, and iii) micron-sized square plates. Further, species-dependent preferences for these morphologies are observed, suggesting potential differences in the profile or concentration of the biochemical constituents in their individual exudates. This data also demonstrates that mycosynthesis of ZnO NPs is independent of the anion species, with nitrate, sulfate, and chloride showing no effect on NP production. Finally, these results enhance the understanding of factors controlling the mycosynthesis of ceramic NPs, supporting future studies that can enable control over the physical and chemical properties of NPs formed through this “green” synthesis method.
Application of X-ray microcomputed tomography in the characterization of irradiated nuclear fuel and material specimens
X-ray microcomputed tomography (µCT) was applied in characterizing the internal structures of a number of irradiated materials, including carbon-carbon fibre composites, nuclear-grade graphite and tristructural isotropic-coated fuel particles. Local cracks in carbon-carbon fibre composites associated with their synthesis process were observed with µCT without any destructive sample preparation. Pore analysis of graphite samples was performed quantitatively, and qualitative analysis of pore distribution was accomplished. It was also shown that high-resolution µCT can be used to probe internal layer defects of tristructural isotropic-coated fuel particles to elucidate the resulting high release of radioisotopes. Layer defects of sizes ranging from 1 to 5 µm and up could be isolated by to-mography. As an added advantage, µCT could also be used to identify regions with high densities of radioisotopes to deter-mine the proper plane and orientation of particle mounting for further analytical characterization, such as materialographic sectioning followed by optical and electron microscopy. Lastly, in fully ceramic matrix fuel forms, despite the highly absorbing matrix, characterization of tristructural isotropic-coated particles embedded in a silicon carbide matrix was accomplished usingµCT and related advanced image analysis techniques.
Development and Deployment Assessment of a Melt-Down Proof Modular Micro Reactor (MDP-MMR)
The objective of this project is to perform feasibility assessment and technology gap analysis and establish a development roadmap for an innovative and highly compact Micro Modular Reactor (MMR) concept that integrates power production, power conversion and electricity generation in a single unit. The MMR is envisioned to use fully ceramic micro-encapsulated (FCM) fuel, a particularly robust form of TRISO fuel, and to be gas-cooled (e.g., He or CO 2 ) and capable of generating power in the range of 10 to 40 MW-thermal. It is designed to be absolutely melt-down proof (MDP) under all circumstances including complete loss of coolant scenarios with no possible release of radioactive material, to be factory produced, to have a cycle length of greater than 20 years, and to be highly proliferation resistant. In addition, it will be transportable, retrievable and suitable for use in remote areas. As such, the MDP-MMR will represent a versatile reactor concept that is suitable for use in various applications including electricity generation, process heat utilization and propulsion.
Novel Use of Water Soluble "Aquapour" As A Temporary Spacer During Coil Winding For The NSTX-U Centerstack
A major facility upgrade to the National Spherical Torus eXperiment (NSTX-U) is currently underway at Princeton Plasma Physics Laboratory (PPPL). A key component of NSTX-U is the fabrication of a new, higher field centerstack (CS). In order to simultaneously provide robust joints between the inner and outer legs of the Toroidal Field Coils (TF) and minimize radial build, the NSTX-U CS design requires that the Ohmic Heating solenoid (OH) be wound directly on the inner TF bundle. To protect the OH against thermal expansion stress during scenarios where the inner TF bundle is hot but the OH is relatively cool, the completed CS will have a 0.100 inch annular gap between the outer diameter of the TF bundle and the inner diameter of the OH solenoid. "Aquapour", a proprietary material produced by the Advanced Ceramics Manufacturing Company will be used during manufacture to produce this gap. After the TF bundle is vacuum pressure impregnated and cured, a cylindrical "clam shell" mold will be assembled around it, and a slurry of powdered Aquapour and water will be pumped into the annular space between the mold and TF bundle. Subsequent baking will turn the Aquapour solid, and a protective layer of wet lay-up fiberglass and resin will be added. The OH solenoid will be wound directly on this wet lay-up shell. After vacuum pressure impregnation of the OH, the water soluble Aquapour will be washed away, leaving the required radial clearance between the TF and OH. This paper will describe prototyping and testing of this process, and plans for use on the actual CS fabrication.
Delamination analysis of metal-ceramic multilayer coatings subject to nanoindentation
Internal damage has been experimentally observed in aluminum (Al)/silicon carbide (SiC) multilayer coatings subject to nanoindentation loading. Post-indentation characterization has identified that delamination at the coating/substrate interface is the most prominent form of damage. In this study the finite element method is employed to study the effect of delamination on indentation-derived hardness and Young's modulus. The model features alternating Al/SiC nanolayers above a silicon (Si) substrate, in consistence with the actual material system used in earlier experiments. Cohesive elements with a traction–separation relationship are used to facilitate delamination along the coating/substrate interface. Delamination is observed numerically to be sensitive to the critical normal and shear stresses that define the cohesive traction–separation behavior. Axial tensile stress below the edge of indentation contact is found to be the largest contributor to damage initiation and evolution. Delamination results in a decrease in both indentation-derived hardness and Young's modulus. As a result, a unique finding is that delamination can occur during the unloading process of indentation, depending on the loading condition and critical tractions.
Falling particle impact erosion testing for particle based CSP systems
CSP systems are currently being examined as an effective method for using solar energy to generate electricity. While much of this research has been conducted using molten salt as the heat transfer medium, in recent years, solid particles have been posited as a cheaper and more energy efficient heat transfer medium for use in CSP systems. Many researchers have looked into the effectiveness of solid particles as a heat transfer medium. However, a concern with the use of particles is that the falling particles will impact various components within the CSP system, such as the hopper, the heat exchanger, and the insulating material, resulting in surface erosion and damage. With repeated impacts from falling particles, material from the surfaces under impact is removed. The degree of erosion depends on whether the substrate is made of brittle or ductile material. Furthermore, factors such as particle shape, size, hardness, concentration, impact angle, particle velocity, and substrate hardness will contribute to the erosion process and determine how much and how quickly erosion will takes place in a system. Three types of erosion will be observed simultaneously: impact erosion from particle impact on receiver, particle storage, and heat exchanger walls, abrasion erosion from particle sliding motion along walls, and attrition erosion as the particles breakdown from particle-to-particle contact and particle-to-wall interactions. It is imperative to understand each of these erosions individually for a more comprehensive understanding and prediction of CSP system durability. In this work, we developed an experimental test setup capable of measuring impact erosion at conditions relevant to 1MW CSP plant. Subsequently, Impact erosion measurements were performed for three different candidate substrate materials at low particle velocities using HSP 40/70 ceramic particles.
Boride-based Ceramic Super-high Temperature Thermocouples in Harsh Environments (Final Scientific/Technical Report)
An electromotive force (emf) can be generated along a temperature gradient between the cold end and hot end of a thermoelectric material, termed the Seebeck effect. Based on the Seebeck effect, metallic alloys have been extensively employed to detect temperatures for centuries, named thermocouples. However, commercially available thermocouple alloys suffer from limitations, such as oxidation, chemical degradation, and poor long-term stability under high-temperature harsh environments. This DOE-funded project aimed to develop high-temperature, chemically tolerant thermocouples suitable for operation in extreme environments relevant to semiconducting thermoelectric materials. The research focused on boride-based semiconducting thermoelectric compounds as candidates for next-generation thermocouples with enhanced oxidation resistance, chemical stability, and thermal robustness under conditions representative of charcoal-fired electricity facilities. During the funded years, boride materials were synthesized using an arc-plasma technique under ambient air and argon atmospheres, enabling scalable and cost-effective production compared with conventional boride fabrication methods. The synthesized borides were processed into nanostructured powders, followed by consolidation into dense bulk materials using a spark plasma sintering (SPS) bottom-up approach. Comprehensive characterization was performed, including microstructural analysis, electrical transport measurements, and optical and thermal property evaluation. Both p-type and n-type boride electric legs were fabricated and integrated into boride-based thermocouples. The thermal and irradiation stabilities of the boride nanomaterials and bulk thermoelectric materials were systematically evaluated to assess suitability for long-term operation in harsh environments. Additionally, 12 students were broadly hands-on trained spanning the full research workflow, including word processing and technical editing (e.g., LATEX for manuscript and poster preparation), data collection and analysis (using Python and related libraries and hardware interfaces), sample preparation (including arc-plasma synthesis and spark plasma sintering), and advanced characterization techniques (such as X-ray diffraction, UV–vis spectroscopy, electron microscopy, differential thermal analysis (DTA), and Seebeck coefficient measurements, etc). Overall, this project demonstrated the feasibility of boride-based thermoelectric materials as durable high-temperature thermocouples, providing a promising pathway toward robust temperature sensing technologies aligned with DOE energy infrastructure and extreme-environment monitoring needs.
A method for evaluating the fatigue crack growth in spiral notch torsion fracture toughness test
The spiral notch torsion test (SNTT) has been a recent breakthrough in measuring fracture toughness for different materials, including metals, ceramics, concrete, and polymers composites. Due to its high geometry constraint and unique loading condition, SNTT can be used to measure the fracture toughness with smaller specimens without concern of size effects. The application of SNTT to brittle materials has been proved to be successful. The micro-cracks induced by original notches in brittle materials could ensure crack growth in SNTT samples. Therefore, no fatigue pre-cracks are needed. The application of SNTT to the ductile material to generate valid toughness data will require a test sample with sufficient crack length. Fatigue pre-crack growth techniques are employed to introduce sharp crack front into the sample. Previously, only rough calculations were applied to estimate the compliance evolution in the SNTT crack growth process, while accurate quantitative descriptions have never been attempted. This generates an urgent need to understand the crack evolution during the SNTT fracture testing process of ductile materials. Here, the newly developed governing equations for SNTT crack growth estimate are discussed in the paper.
Neutron reflectometry investigations of interfacial structures of Ti/TiN layers deposited by magnetron sputtering
We report that nanolayered metal-ceramic composite systems provide the possibility to produce new materials with exceptional strength, toughness, and radiation resistance not exhibited by their individual constituents. The unusual behaviors are frequently attributed to the high density of internal interfaces. Most layered structures studied to date contain sharp interfaces and the synthesis of more diffuse interfacial structures, where the interface is graded out of the interface plane, has not been deeply explored. Here we show how neutron reflectometry was used to study the structure of magnetron sputter deposited titanium and titanium nitride (Ti/TiN) layers as a function of deposition parameters: temperature, rate of N 2 flow or pressure, electrical bias applied to the sample, and orientation of the ion source relative to the sample. These different deposition and post-processing strategies resulted in profound changes in the structure of the interfacial region between the two components in Ti/TiN x bilayers. Finally, the results show that temperature and low step-wise N 2 flow rates, but not electrical bias, can form graded interfaces in a controlled manner.
New portable instrument for the measurement of thermal conductivity in gas process conditions
The development of high temperature gas sensors for the monitoring and determination of thermophysical properties of complex process mixtures at high temperatures faces several problems, related with the materials compatibility, active sensing parts sensitivity, and lifetime. Ceramic/thin metal films based sensors, previously developed for the determination of thermal conductivity of molten materials up to 1200 °C, were redesigned, constructed, and applied for thermal conductivity measuring sensors. Platinum resistance thermometers were also developed using the same technology, to be used in the temperature measurement, which were also constructed and tested. A new data acquisition system for the thermal conductivity sensors, based on a linearization of the transient hot-strip model, including a portable electronic bridge for the measurement of the thermal conductivity in gas process conditions was also developed. The equipment is capable of measuring the thermal conductivity of gaseous phases with an accuracy of 2%-5% up to 840 °C (95% confidence level). The development of sensors up to 1200 °C, present at the core of the combustion chambers, will be done in a near future.
Low Impedance Cathode/Electrolyte Interfaces for High Energy Density Solid-State Batteries
All-solid-state batteries (ASSBs) using a ceramic fast Li-ion conductor as a solid-state electrolyte (SSE) have been proposed as a promising strategy to significantly increase the energy density of lithium batteries. Due to their high ion conductivity and excellent stability, Li-stuffed garnets exhibit the most promising physical and chemical properties for SSEs. However, the typical microstructure, thick (>100 μm) bulk electrolyte and simple planar electrode/electrolyte interfaces, combined with poor electrode wetting of the garnet result in excessively high area specific resistances (ASRs) that severely limit achievable current density and cell energy density. In this project, the team is building on their demonstrated expertise with garnet electrolytes and ASSBs to accomplish the following: (1) engineer interfaces to overcome high NMC/LLZ interfacial impedance and interfacial degradation; (2) develop processing and fabrication techniques to achieve high loading NMC/LLZ composite cathodes with low resistance and high cyclability; and (3) integrate the NMC/LLZ cathodes into all-solid-state Li-metal/LLZ cells to achieve high-energy-density batteries.
The synthesis and electrical transport properties of carbon/Cr 2 GaC MAX phase composite microwires
While MAX phases offer an exotic combination of ceramic and metallic properties, rendering them a unique class of materials, their applications remain virtually hypothetical. To overcome this shortcoming, a sol–gel based route is introduced that allows access to microwires in the range of tens of micrometers. Thorough structural characterization through XRD, SEM, EDS, and AFM demonstrates a successful synthesis of carbonaceous Cr2GaC wires, and advanced low temperature electronic transport measurements revealed resistivity behavior dominated by amorphous carbon. Here, the tunability of electronic behavior of the obtained microwires is shown by a halide post-synthesis treatment, allowing purposeful engineering of the microwires’ electrical conductivity. Raman studies revealed the polyanionic nature of the intercalated halides and a slow decrease in halide concentration was concluded from time-dependent conductivity measurements. Based on these findings, the process is considered a viable candidate for fabricating chemiresistive halogen gas sensors.
Fabrication of UN-Mo CERMET Nuclear Fuel Using Advanced Manufacturing Techniques
Ceramic-metallic nuclear fuels are a candidate fuel for nuclear thermal propulsion systems due to their high heat transport properties, which are necessary in very high-temperature environments. The conventional fabrication of uranium nitride–molybdenum fuel has been thoroughly studied in the past, but modern manufacturing techniques have presented a unique opportunity for further development within this field. This work demonstrates the use of advanced manufacturing techniques to produce nuclear fuel pellets composed of uranium nitride microspheres encased in a molybdenum matrix. Binder jetting is used to print molybdenum disks that are filled with uranium nitride microspheres and afterward sintered using spark plasma sintering. Two fuel pellets were fabricated to demonstrate the methodology and to provide a baseline analysis of the effects of temperature and pressure processing conditions. Characterization of the sintered fuel pellets includes detailed microstructural analysis and thermal conductivity measurements.
Cracking during pyrolysis of preceramic polymers within glass microtubes
Abstract Cracking of preceramic polymers during pyrolysis under highly‐constrained conditions is examined by X‐ray computed tomography of fine glass microtubes containing the pyrolyzing material. The microtubes represent model geometries that mimic the long channels between fibers during production of ceramic composites by precursor impregnation and pyrolysis. Complementary fracture mechanics analyses of interface cracking and crack kinking are used to glean insights into the conditions under which periodic alternating cracks form. A key finding is that alternating cracks are an inherent feature of constrained pyrolysis . This feature is attributable in large part to the high energy release rates for interface cracks to kink into the pyrolyzing material under the hydrostatic tension developed during pyrolysis. It also requires interfaces with toughness comparable to that of the pyrolyzing material, to prevent large‐scale interface separation. The results further indicate the need for small uniform spaces for pyrolysis within fiber preforms in order to produce networks of fine periodic pyrolysis cracks; these networks in turn facilitate impregnation and pyrolysis in subsequent processing cycles.
Numerical Simulation of Container Breach and Airborne Release of Solids Due to Mechanical Insults
Throughout U.S. Department of Energy (DOE) complexes, safety engineers employ the five-factor formula to calculate the source term (ST) that includes parameters of airborne release fraction (ARF), respirable fraction (RF) and damage ratio (DR). Limited experimental data on fragmentation of solids, such as ceramic pellets (i.e., PuO2), and container breach due to mechanical insults (i.e., drop and forklift impact), can be supplemented by modeling and simulation using high fidelity computational tools to estimate these parameters. This paper presents the use of Sandia National Laboratories' SIERRA solid mechanics (SM) finite element code to investigate the behavior of the widely utilized waste container (such as 7A Drum) subject to a range of free fall impact and puncture scenarios. The resulting behavior of the container is assessed, and the estimates are presented for bounding DRs from calculated breach areas for the various accident conditions considered. This paper also describes a novel multiscale constitutive model recently implemented in SIERRA/SM that simulates the fracture of brittle materials such as PuO 2 and determines ARF during the fracture process. Furthermore, comparisons are made between model predictions and simple bench-top experiments.
Wettability, structural and optical properties investigation of TiO{sub 2} nanotubular arrays
Graphical abstract: FESEM images of the TiO 2 nanotube layers formed at 0.5 wt% NH4F/ glycerol. - Highlights: • Structural property investigation of TiO{sub 2} nanotube. • Evaluation of wettability of TiO{sub 2} nanotube. • Study on optical properties of TiO{sub 2} nanotube. • The effect of anatase phase on optical and wettability properties of TiO{sub 2.} - Abstract: In this study, the effect of microstructural evolution of TiO{sub 2} nanotubular arrays on wettability and optical properties was investigated. Pure titanium was deposited on silica glass by PVD magnetron sputtering technique. The Ti coated substrates were anodized in an electrolyte containing NH{sub 4}F/glycerol. The structures of the ordered anodic TiO{sub 2} nanotubes (ATNs) as long as 175 nm were studied using field emission scanning electron microscopy (FESEM) and X-ray diffraction (XRD). The result shows a sharp peak in the optical absorbance spectra around the band gap energy, 3.49–3.42 eV for annealed and non-annealed respectively. The thermal process induced growth of the grain size, which influence on the density of particles and the index of refraction. Furthermore, the wettability tests' result displays that the contact angle of intact substrate (θ = 74.7°) was decreased to 31.4° and 17.4° after anodization for amorphous and heat treated (450 °C) ANTs coated substrate, respectively.