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At least 865 records · Page 48

Durability of Ceramic Matrix Composites in Combustion Environments

SiO2 scale volatility and the resulting recession of SiC has been previously identified for CVD, as well as sintered, SiC and Si3N4 materials. Linear weight loss and surface recession of SiC was observed as a result of SiO2 volatility for both fuel-lean and fuel-rich gas mixtures. A strong Arrhenius temperature dependence exist and parametric studies using multiple linear regression were used to develop recession relationships as a function of e(sup -Q/RT) central dot P(sup X)V(sup y) for both lean and rich combustion conditions. Recession of 0.2 - 2.0 micron/hr is predicted for typical combustion conditions at 1200 - 1400 C, with a somewhat higher absolute recession rate and activation energy for rich combustion versus lean.

Robinson, Raymond C.↗

Diffusion Bonding of Silicon Carbide Ceramics using Titanium Interlayers

Robust joining approaches for silicon carbide ceramics are critically needed to fabricate leak free joints with high temperature mechanical capability. In this study, titanium foils and physical vapor deposited (PVD) titanium coatings were used to form diffusion bonds between SiC ceramics using hot pressing. Silicon carbide substrate materials used for bonding include sintered SiC and two types of CVD SiC. Microscopy results show the formation of well adhered diffusion bonds. The bond strengths as determined from pull tests are on the order of several ksi, which is much higher than required for a proposed application. Microprobe results show the distribution of silicon, carbon, titanium, and other minor elements across the diffusion bond. Compositions of several phases formed in the joint region were identified. Potential issues of material compatibility and optimal bond formation will also be discussed.

Halbig, Michael C.↗

High density UO 2 and high thermal conductivity UO 2 composites by spark plasma sintering (SPS)

Embodiments of the invention are directed to a method for production of a nuclear fuel pellet by spark plasma sintering (SPS), wherein a fuel pellet with more than 80% TD or more than 90% TD is formed. The SPS can be performed with the imposition of a controlled uniaxial pressure applied at the maximum temperature of the processing to achieve a very high density, in excess of 95% TD, at temperatures of 850 to 1600° C. The formation of a fuel pellet can be carried out in one hour or less. In an embodiment of the invention, a nuclear fuel pellet comprises UO 2 and a highly thermally conductive material, such as SiC or diamond.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

High density UO2 and high thermal conductivity UO2 composites by spark plasma sintering (SPS)

Embodiments of the invention are directed to a method for production of a nuclear fuel pellet by spark plasma sintering (SPS), wherein a fuel pellet with more than 80% TD or more than 90% TD is formed. The SPS can be performed with the imposition of a controlled uniaxial pressure applied at the maximum temperature of the processing to achieve a very high density, in excess of 95% TD, at temperatures of 850 to 1600° C. The formation of a fuel pellet can be carried out in one hour or less. In an embodiment of the invention, a nuclear fuel pellet comprises UO 2 and a highly thermally conductive material, such as SiC or diamond.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Ultra-high temperature carbide foams and methods of fabricating the same

Ultra-high temperature carbide (UHTC) foams and methods of fabricating and using the same are provided. The UHTC foams are produced in a three-step process, including UHTC slurry preparation, freeze-drying, and spark plasma sintering (SPS). The fabrication methods allow for the production of any kind of single- or multi-component UHTC foam, while also providing flexibility in the shape and size of the UHTC foams to produce near-net-shape components.

Agarwal, Arvind↗

Ultra-high temperature carbide foams and methods of fabricating the same

Ultra-high temperature carbide (UHTC) foams and methods of fabricating and using the same are provided. The UHTC foams are produced in a three-step process, including UHTC slurry preparation, freeze-drying, and spark plasma sintering (SPS). The fabrication methods allow for the production of any kind of single- or multi-component UHTC foam, while also providing flexibility in the shape and size of the UHTC foams to produce near-net-shape components.

Agarwal, Arvind↗

Methods and apparatus for improved thermal monitoring by correlating infrared emissivity to surface topography

Embodiments of the present disclosure provide an improved method and apparatus for thermal monitoring for a metal additive manufacturing system. An emissivity value of a top surface of an object to be manufactured is determined based, at least in part, on an arithmetic product of a predetermined roughness value and a predetermined slope-related value. The predetermined roughness value and slope-related values are predetermined based, at least in part, on measurements of a previously manufactured object. The system sinters a metal to form the top surface of the object to be manufactured. An infrared sensor detects radiation from at least a portion of the top surface of the object to be manufactured. A temperature is generated based, at least in part, on the detected infrared radiation and the emissivity value and the generated temperature is applied to a temperature utilization component of the system.

Taylor, Samantha↗

Spark plasma sintering (SPS) densified U 3 Si 2 pellets: Microstructure control and enhanced mechanical and oxidation properties

Dense U 3 Si 2 pellets with controlled grain structure and enhanced thermal-mechanical and oxidation properties are synthesized with spark plasma sintering (SPS). Microstructure and phase composition of the SPS densified pellets are characterized systematically using SEM, EDS, and XRD. Thermal-mechanical properties and oxidation behavior of the sintered silicide fuel pellets are analyzed by laser flash, indentation, and dynamic thermogravimetric analysis. Dense U 3 Si 2 pellets are consolidated by combining high energy ball milling and rapid sintering by SPS, and the microstructure structures are controlled from micron-sized (~5.7 μm grain size) for conventional silicide to a nanocrystalline matrix with an average grain size of ~280 nm. A dominant phase of distorted U 3 Si 2 was identified with lattice expansion due to residual thermal stress upon SPS consolidation and rapid cooling processes. Both micron-sized and nano-sized pellets show exceptional thermal transport properties, consistent with monolithic silicides reported in literature. The SPS-densified pellets possess simultaneously high hardness and fracture toughness. The SPS-densified silicide pellets also demonstrate exceptional oxidation performance with extended onset oxidation temperature above 500 °C and reduced oxidation kinetics, particularly for nano-sized pellets. A strong strain effect was proposed in which compressive stress in nano-sized pellets enhances the oxidation resistance of silicide fuels, as evidenced by the degradation of oxidation performance upon strain relaxation by isothermal annealing. The correlation among the sintering process – microstructure control – physical properties and fuel behavior is established. A new concept of strain engineering is proposed further properties optimization, enabling the development of potential oxidation and corrosion-resistant silicides with extended performance, the key technological challenge of U 3 Si 2 as the leading concept of accident tolerant fuels.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Post Examination of Candidate NpO 2 Targets for 238 Pu Production

Four targets composed of sintered NpO 2 pellets enclosed in Zircaloy cladding were irradiated in the High Flux Isotope Reactor for 2 to 4 cycles to determine if an oxide pellet and Zircaloy cladding would be usable candidates for 238 Pu production. The pellets were sintered to a high fraction of theoretical density (TD) and melt wires were placed in small holes that had been drilled in the center of selected pellets to determine if the pellet centers exceeded desirable operating temperatures. After irradiation, the targets were punctured to determine the internal target pressure and the fission gas release. None of the targets had excessive pressure, and fission gas release was in the range of 4 to 38%. The targets were then cut into segments for radiochemical analysis, and metallography (MET) mounts were created to examine the pellet microstructure and to search for the melt wires to determine if they had melted. Three of the four targets resulted in successful MET mounts; the two-cycle pellets were too friable to be handled. No signs of pellet melting were noted, and unfortunately, none of the melt wires could be recovered. The results indicate that this pellet/clad design offers a practical option for 238 Pu production.

36 MATERIALS SCIENCE↗

Development of Advanced Low Conductivity Thermal Barrier Coatings

Advanced multi-component, low conductivity oxide thermal barrier coatings have been developed using an approach that emphasizes real-time monitoring of thermal conductivity under conditions that are engine-like in terms of temperatures and heat fluxes. This is in contrast to the traditional approach where coatings are initially optimized in terms of furnace and burner rig durability with subsequent measurement in the as-processed or furnace-sintered condition. The present work establishes a laser high-heat-flux test as the basis for evaluating advanced plasma-sprayed and electron beam-physical vapor deposited (EB-PVD) thermal barrier coatings under the NASA Ultra-Efficient Engine Technology (UEET) Program. The candidate coating materials for this program are novel thermal barrier coatings that are found to have significantly reduced thermal conductivities and improved thermal stability due to an oxide-defect-cluster design. Critical issues for designing advanced low conductivity coatings with improved coating durability are also discussed.

Zhu, Dong-Ming↗

Hot Hydrogen Testing of Uranium Nitride Cermet for Nuclear Thermal Propulsion

This study investigated the thermochemical stability and performance characteristics of uranium mononitride tungsten molybdenum cermet (UN-Mo30W) as a potential fuel material for Nuclear Thermal Propulsion (NTP) engines. Twelve monolithic cylinders were subjected to conditions simulating an active NTP engine. The tests demonstrated thermal variability within the test article and highlighted the dissociation of UN into U and N2 at elevated temperatures, affecting the microstructure and causing bonding between cermet wafers and cooling tubes. Findings indicate that while UN-Mo30W cermet exhibits some desirable properties for NTP applications, its suitability is limited by high-temperature thermochemical instability.

nuclear fuels↗

Process for fabrication of enhanced β″-alumina solid electrolytes for energy storage devices and energy applications

A dense β″-alumina/zirconia composite solid electrolyte and process for fabrication are disclosed. The process allows fabrication at temperatures at or below 1600° C. The solid electrolytes include a dense composite matrix of β″-alumina and zirconia, and one or more transition metal oxides that aid the conversion and densification of precursor salts during sintering. The composite solid electrolytes find application in sodium energy storage devices and power-grid systems and devices for energy applications.

Lu, Xiaochuan↗

Imaging of Calibrated Defects in Additively Manufactured Materials: Pulsed Thermal Tomography Nondestructive Examination of Additively Manufactured Reactor Materials and Components

Additive manufacturing (AM, or 3D printing) for commercial nuclear energy applications is an emerging method for cost-efficient manufacturing aimed at replacing aging nuclear reactor parts and reducing costs for new construction. Known material flaws in AM include low-density regions consisting of non-sintered powder, which have to be detected to ensure the safety of long-term performance nuclear reactor components. Currently, limited options are available for nondestructive evaluation (NDE), either during or post manufacturing. As a solution to NDE of AM, we are developing pulsed thermal imaging which is non-contact, one-sided, and scalable to arbitrary size and shape of the AM parts. Pulsed thermography (PT) system utilizes a high intensity flash lamp to rapidly heat surface of sample, and a high sensitivity fast-frame megapixel infrared (IR) camera to capture data of surface temperature variations. The acquired data cube consists of a stack of surface temperature images taken at different times. Information about material internal defects is extracted by analyzing the data cube. This report provides results of preliminary performance evaluation of pulsed thermal imaging capability in detection of imprinted flaws in AM metallic structures. The flaws were introduced into AM parts as imprinted hemispherical low density regions, consisting of trapped un-sintered metallic powder. Specimens for developed for this study consisted of AM stainless steel 316 and Inconel 718 plates. The diameters of imprinted defects varied from 1mm to 8mm, and their depths below the plate flat surface varied between 1mm and 6mm. Pulsed thermal tomography (PTT) processes the measured data cube to obtain 3D reconstructions of material effusivity using a unique inversion algorithm developed at Argonne. PTT has been previously used in imaging of similar size flat bottom hole (FBH) simulated defects in stainless steel 316 and Inconel 718 specimens. In the study involving AM specimens, PTT imaging results have shown that 1mm-diameter defects located 1mm and 2mm below the surface of specimens were detectable. Larger size defects were detectable at greater depth. We also explored an alternative approach to detection of material flaws in PT data cube, which is using neural learning-based approach to blind source separation. Detection of small material defects requires finding features in the data cube which have signal contrast levels approaching sensitivity limit of IR camera. In this study, an optimized Neural Learning based Blind Source Separation (NLBSS) algorithm, including Principal Component Analysis (PCA), and Independent Component Analysis (ICA) is demonstrated to automatically extract principal temporal and spatial features of thermography frames to enhance flaw detection. By using the NLBSS algorithm, material internal defects can be automatically detected. Furthermore, this processing approach compensates for experimental thermal imaging artifacts, such as noise and uneven heating. By merging artificial intelligence with phtotothermics, the NDE system detects internal calibrated defects of various sizes and depths in AM nuclear-grade metallic alloys.

36 MATERIALS SCIENCE↗

Photonic curing for innovative fabrication of flexible metal oxide optoelectronics

Abstract Flexible optoelectronics, based on non-planar substrates, hold promise for diverse applications such as wearables, health monitors, and displays due to their cost-effective manufacturing methods. Despite the superior properties of metal oxides, the challenge of processing them at high temperatures incompatible with plastic substrates necessitates innovative annealing approaches. Photonic curing, which delivers microsecond to millisecond broadband (200–1500 nm) light pulses on a sample, emerges as a viable solution. Depending on the optical properties, the targeted film absorbs the radiant energy resulting in rapid heating while the transparent substrate absorbs a minimal amount of light and remains at ambient temperature. The light intensity can be high, but since the light pulse is short, the total energy absorbed by the sample remains low and will not damage the plastic substrate. This perspective explores the innovative application of photonic curing to fabricate flexible metal oxide optoelectronics, including thin-film transistors, metal–insulator–metal devices, solar cells, transparent conductors, and Li batteries, emphasizing the conversion of sol–gel precursors to metal oxides. However, this technique was initially developed for sintering metal nanoparticles to conductive patterns and poses intriguing challenges in explaining its mechanism for metal oxide conversion, especially considering the limited absorption of visible light by most sol–gel precursors. The review delves into UV-induced photochemistry, common flexible metal-oxide optoelectronic components, and non-intuitive distinctions between photonic curing and thermal annealing. By elucidating the distinctive role of photonic curing in overcoming temperature-related challenges and advancing the fabrication of flexible metal oxide optoelectronics, this perspective offers valuable insights that could shape the future of flexible optoelectronics.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

Multiscale Porous High-temperature Heat Exchanger Using Ceramic Co-extrusion

In this project, our MIT, Purdue, and GE team aims to design, model, fabricate, and test a novel high temperature, compact, and durable ceramic heat exchanger to be operated under high temperature and pressure conditions for aerospace applications. Our approach is grounded in introducing multiscale porosity, i.e., centimeter-scale channels embedded with micrometer-scale channels, into the ceramic heat exchanger to significantly improve its heat transfer performance and mechanical strength while maintaining minimal pressure losses. We first developed high-fidelity thermal-fluid-mechanical model capable of precisely capturing the heat transfer rate, temperature profile, pressure drop, and mechanical stress throughout the entire heat exchanger design. Guided by our model, we identified the optimal design parameters for the SiC heat exchanger body and manifolds. Then, we established a completed fabrication procedure to create multiscale features in the ceramic heat exchanger, including co-extrusion, lamination, burnout, and sintering. We fabricated multiple heat exchanger bodies consisting of 6 × 6 and 3 × 3 centimeter-scale channels where each individual centimeter-scale channel comprises 625 crack-free microchannels with 90 μm × 90 μm opening. Owing to the multiscale features, our fabricated heat exchanger bodies exhibited desirable mechanical strength with 156 MPa flexural strength under 1300 Celsius degree. Despite the demonstrated highly tailorable microscopic features and superior mechanical strength, we identified delamination due to the complex interaction among ceramic, polymer, and gas species can be a critical challenge to create fully defect-free heat exchanger, which requires further fundamental investigations in future works. To test the heat exchanger performance, we constructed a high-temperature and high-pressure experimental apparatus that can be safely operated under 400 Celsius degree and 4 bar. With insights gained from mechanistic modeling, material development, and detailed characterization, a cost model was finally developed to understand the market potential of the developed technology, where a cost of $43,000 Celsius degree/kW was envisioned. This project developed a transformative approach to high-performance heat exchanger design. The thermal-fluid-mechanical design approach developed in this project can serve as a generic tool to guide the design of various heat-exchangers operated under high-temperature and high-pressure conditions. The material fabrication approach established in this project can be a useful guide for ceramic processing at extreme length scales.

42 ENGINEERING↗

Unveiling enhanced oxidation resistance and mechanical integrity of multicomponent ultra–high temperature carbides

The development of a new class of multicomponent ultra-high temperature ceramics (MC-UHTCs), often referred to as high-entropy UHTCs, has gained increased interest due to the possibility of improved thermomechanical and oxidation properties. In this study, a systematic approach by gradual addition in the UHTC components ranging from a binary to a dense quaternary (Ta,Nb,Hf,Ti)C is synthesized using spark plasma sintering (SPS). The solid solutioning was the critical factor in homogenizing the composition in the multicomponent system. The segregation of NbC and HfC was seen in binary and ternary UHTC systems, while a single-phase homogeneity was observed in the quaternary UHTC improving its hardness up to 34.8 GPa. The presence of closely spaced slip lines in the MC-UHTCs enhances resistance to indentation damage up to 72% at an applied load of 200 N. The formation of complex mixed oxide phase of Hf6Ta2O17 ensued in the lower to negligible oxidation even up to 3 min of plasma exposure with temperature exceeding 2800°C. In sum, though the entropy remains medium (0.96R) for the selected system, the quaternary UHTC system undoubtedly has significantly better thermomechanical performance when compared to established baseline UHTCs. Furthermore, this raises the debate on the justification for calling a multicomponent system a “high entropy” to be seen in a new light. The developed MC-UHTCs elicits the paradigm of this new class of UHTCs expanding their potential in thermal protection systems for hypersonic applications.

36 MATERIALS SCIENCE↗

Investigation of MgO additives on microstructure and properties of thin LLZO electrolytes for all-solid-state batteries

To realize high-energy density lithium lanthanum zirconate (LLZO)-based solid-state batteries (SSB), LLZO electrolytes should be fabricated with low thickness and high mechanical strength. An effective strategy for strengthening ceramic materials is to use additives. Here, we employed MgO nanopowders and fibers as additives for the thin LLZO electrolyte in order to improve the mechanical strength. The microstructure, mechanical properties, and electrochemical properties are characterized to investigate the effects of adding MgO and sintering time. The MgO remains at grain boundaries after sintering, making the microstructure of LLZO fine and uniform. The mechanical strength of the MgO-added LLZO was enhanced by more than 60% while maintaining high ionic conductivity (1 × 10 -4 S cm -1 ) at room temperature. Li symmetric cells using the MgO fiber–LLZO and MgO powder–LLZO exhibit 2 and 3 times higher critical current density (CCD) than those of pure LLZO, and a solid-state full cell exhibits stable cycling performance. Further, these results demonstrate that the use of MgO nanopowder or fiber as an additive for thin LLZO is beneficial for high-current density cycling, by improving mechanical properties and microstructure.

25 ENERGY STORAGE↗

Sintering and hot pressing of Fra Mauro composition glass and the lithification of lunar breccias.

It is proposed that Apollo 14 type breccias lithify by sintering of particles of matrix glass under stress-free conditions. Meteorite impacts generate the heat necessary for sintering. Compacted angular particles of glass with the composition of an Apollo 14 rock were sintered experimentally. Loose clods of sub 37 micron grains form in several days at 700 C. Synthetic rocks, which texturally resemble the breccias, were produced at 795 C and above in 7.5 hours. Glass devitrified with increasing temperature. At 850 C, devitrification prevents much further densification of the synthetic breccias after 2 hours. Experiments compressing glass at 500 bars at 600 C produced dense vitreous masses which did not resemble lunar breccias. Confining pressure does not play a major role in lithifying the breccias. It is concluded that Apollo 14 type lunar breccias form at shallow depths at 800 C+ in a period of minutes to days.

Simonds, C. H.↗