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At least 361 records · Page 20

Final Test Results for the Ground Operations Demonstration Unit for Liquid Hydrogen

Described herein is a comprehensive project—a large-scale test of an integrated refrigeration and storage system called the Ground Operations and Demonstration Unit for Liquid Hydrogen (GODU LH2), sponsored by the Advanced Exploration Systems Program and constructed at Kennedy Space Center. A commercial cryogenic refrigerator interfaced with a 125,000 liter liquid hydrogen tank and auxiliary systems in a manner that enabled control of the propellant state by extracting heat via a closed loop Brayton cycle refrigerator coupled to a novel internal heat exchanger. Three primary objectives were demonstrating zero-loss storage and transfer, gaseous liquefaction, and propellant densification. Testing was performed at three different liquid hydrogen fill-levels. Data were collected on tank pressure, internal tank temperature profiles, mass flow in and out of the system, and refrigeration system performance. All test objectives were successfully achieved during approximately two years of testing. A summary of the final results is presented in this paper.

Zero Boil Off↗

Effect of pelleting on the recalcitrance and bioconversion of dilute-acid pretreated corn stover

Background: Knowledge regarding the performance of densified biomass in biochemical processes is limited. The effects of densification on biochemical conversion are explored here. Methods: Pelleted corn stover samples were generated from bales that were milled to 6.35 mm. Low-solids acid pretreatment and simultaneous saccharification and fermentation were performed to evaluate pretreatment efficacy and ethanol yields achieved for pelleted and ground stover (6.35 mm and 2 mm) samples. Both pelleted and 6.35-mm ground stover were evaluated using a ZipperClave® reactor under high-solids, process-relevant conditions for multiple pretreatment severities (Ro), followed by enzymatic hydrolysis of the washed, pretreated solids. Results: Monomeric xylose yields were significantly higher for pellets (approximately 60%) than for ground formats (approximately 38%). Pellets achieved approximately 84% of theoretical ethanol yield (TEY); ground stover formats had similar profiles, reaching approximately 68% TEY. Pelleting corn stover was not detrimental to pretreatment efficacy for both low- and high-solids conditions, and even enhanced ethanol yields.

09 BIOMASS FUELS↗

Are the U.S. Biorefineries Over the Hurdle of 2000 Ton Daily Throughput Yet?

The efficient utilization of lignocellulosic biomass for biofuel and biochemical production is hindered by material handling issues such as clogging and segregation among other challenges. Preprocessing methods such as drying, screening, and milling have improved conversion yield but have not sufficiently enhanced flowability, especially herbaceous biomass. The poor flowability of herbaceous biomass is rooted in some particle attributes that remain less altered by those methods, e.g., irregular particle shape, high roughness, and high compressibility, making it hard to scale up throughput to a key benchmark for a biorefinery – 2000 ton per day. Applying additional preprocessing methods like pelletization and torrefaction to drastically change those particle attributes can improve flow and handling but has not been comprehensively verified through test. The flowability of herbaceous biomass feedstock formats generated by three different preprocessing methods was recently assessed at Idaho National Laboratory’s Biomass Feedstock National User Facility: first, loose particles size reduced from as-received materials; second, pellets produced from an efficient densification process; and third, powders milled from torrefied pellets. Benchmarking tests including static angle of repose, basic flow energy measured in a powder rheometer, and discharge flow in an adjustable hopper, were conducted to evaluate those feedstock formats. Beyond the capacity of existing experimental apparatuses, a digital engineering approach involving flow simulations and AI models were used to identity the material attributes and processing parameters that have dominant influences on flow throughput. Techno-economic analysis focusing on hopper flow as a typical material handling operation was conducted for those feedstock formats. Perspectives will be discussed on whether the 2000-ton daily throughput for a biorefinery is achievable at an acceptable cost by using any of the tested preprocessing methods.

09 - BIOMASS FUELS↗

FUNCTIONALIZED SILICA AEROGELS: ADVANCED MATERIALS TO CAPTURE AND IMMOBILIZE RADIOACTIVE IODINE

To support the future expansion of nuclear energy, an effective method is needed to capture and safely store radiological iodine-129 released during reprocessing of spent nuclear fuel. Various materials have been investigated to capture and immobilize iodine. In most cases, however, the materials that are effective for capturing iodine cannot subsequently be sintered/densified to create a stable composite that could be a viable waste form. We have developed chemically modified, highly porous, silica aerogels that show sorption capacities higher than 440 mg of I2 per gram at 150 C. An iodine uptake test in dry air containing 4.2 ppm of iodine demonstrated no breakthrough after 3.5 h and indicated a decontamination factor in excess of 310. Preliminary densification tests showed that the I2-loaded aerogels retained more than 92 wt% of I2 after thermal sintering with pressure assistance at 1200 C for 30 min. These high capture and retention efficiencies for I2 can be further improved by optimizing the functionalization process and the chemistry as well as the sintering conditions.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Sintering behavior of Lanthana-bearing nanostructured ferritic steel consolidated via spark plasma sintering

Elemental powder mixture of Fe–14Cr–1Ti–0.3Mo–0.5La 2 O 3 (wt%) composition is mechanically alloyed for different milling durations (5, 10 and 20 h) and subsequently consolidated via spark plasma sintering under vacuum at 950 °C for 7 min. The effects of milling time on the densification behavior and density/microhardness are studied. The sintering activation energy is found to be close to that of grain boundary diffusion. The bimodal grain structure created in the milled and sintered material is found to be a result of milling and not of sintering alone. The oxide particle diameter varies between 2 and 70 nm. As a result, faceted precipitates smaller than 10 nm in diameter are found to be mostly La–Ti–Cr-enriched complex oxides that restrict further recrystallization and related phenomena.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Acetabular Cup with a Trabecular Coating: A Novel Approach to a Monolithic Cup Made of One High-Strength Ceramic Material

An advanced monolithic cup comprising a thin liner and a trabecular coating is a promising alternative to the current modular ceramic cups for hip replacements because it can be anchored directly to the human bone and features larger femoral heads allowing a greater range of motion. In this study, the authors propose a fabrication route for an advanced monolithic cup of only one high-strength ceramic material by joining a partially sintered liner and a coating with a ceramic paste as an intermediate layer and subsequent sintering. Therefore, the challenge here is to avoid the formation of defects at the coating/intermediate layer interfaces during classical sintering which is due to compressive tension constrained coating sintering in the initial sintering stages. In this study, the defect formation is minimized by sintering at constant low shrinkage rates, as this results in favorable compressive stresses in the coating in the initial sintering stages and a decrease in the differences in the densification rates. For the first time, by using the proposed route, the authors prepare an advanced monolithic cup of only alumina-toughened zirconia (ATZ) that contains a coating with a porosity of 50 vol% and interconnected pores between 150 and 450 μm, as required for bone-ingrowth.

36 MATERIALS SCIENCE↗

Cold Sintering Process of Composites: Bridging the Processing Temperature Gap of Ceramic and Polymer Materials

Co-sintering ceramic and thermoplastic polymer composites in a single step with very high volume fractions of ceramics seems unlikely, given the vast differences in the typical sintering temperatures of ceramics versus polymers. These processing limitations are overcome with the introduction of a new sintering approach, namely “cold sintering process” (CSP). CSP utilizes a transient low temperature solvent, such as water or water with dissolved solutes in stoichiometric ratios consistent with the ceramic composition, to control the dissolution and precipitation of ceramics and effect densification between room temperature and ≈200 °C. Under these conditions, thermoplastic polymers and ceramic materials can be jointly formed into dense composites. Three diphasic composite examples are demonstrated to show the overall diversity of composite material design between organic and inorganic oxides, including the microwave dielectric Li 2 MoO 4 –(-C 2 F 4 -) n , electrolyte Li 1.5 Al 0.5 Ge 1.5 (PO 4 ) 3 –(-CH 2 CF 2 -) x [-CF2CF(CF3)-] y, and semiconductor V 2 O 5 –poly(3,4-ethylenedioxythiophene) polystyrene sulfonate composites. Cold sintering is more general and shall have a major impact on the processing of composite materials for many different applications, mechanical, thermal, and electronic, to mention a few possibilities. CSP concepts open up new composite material design and device integration schemes, impacting a wide variety of applications.

36 MATERIALS SCIENCE↗

Ultra‐Uniform Nanocrystalline Materials via Two‐Step Sintering

Abstract Nanocrystalline materials with superior properties are of great interest. Much is discussed about obtaining nanograins, but little is known about maintaining grain‐size uniformity that is critical for reliability. An especially intriguing question is whether it is possible to achieve a size distribution narrower than what Hillert theoretically predicted for normal grain growth, a possibility suggested—for growth with a higher growth exponent—by the generalized mean‐field theory of Lifshitz, Slyozov, Wagner (LSW), and Hillert but never realized in practice. Following a rationally designed two‐step sintering route, it has been made possible in bulk materials by taking advantage of the large growth exponent in the intermediate sintering stage to form a uniform microstructure despite residual porosity, and freezing the grain growth thereafter while continuing densification to reach full density. The bulk dense Al 2 O 3 ceramic thus obtained has an average grain size of 34 nm and a size distribution much narrower than Hillert's prediction. Bulk Al 2 O 3 with a grain‐size distribution narrower than the particle‐size distribution of starting powders is also demonstrated, as are highly uniform bulk engineering metals (refractory Mo and W‐Re alloy) and complex functional ceramics (BaTiO 3 ‐based alloys with superior dielectric strength and energy capacity).

Dong, Yanhao↗

In Situ Construction of Uniform and Robust Cathode–Electrolyte Interphase for Li-Rich Layered Oxides

The high-energy-density Li-rich layered oxides (LLOs) as promising cathodes for Li-ion batteries suffer from the dissolution of transition metals (especially manganese) and severe side reactions in conventional electrolytes, which greatly deteriorate their electrochemical performance. Herein, an in situ “anchoring + pouring” synergistic cathode-electrolyte interphase (CEI) construction is realized by using 1,3,6-hexanetricarbonitrile (HTCN) and tris(trimethylsilyl) phosphate (TMSP) electrolyte additives to alleviate the challenges of an LLO (Li 1.13 Mn 0.517 Ni 0.256 Co 0.097 O 2 ). HTCN with three nitrile groups can tightly anchor transition metals by coordinative interaction to form the CEI framework, and TMSP will electrochemically decompose to reshape the CEI layer. The uniform and robust in situ constructed CEI layer can suppress the transition metal dissolution, shield the cathode against diverse side reactions, and significantly improve the overall electrochemical performance of the cathode with a discharge voltage decay of only 0.5 mV/cycle -1 . Further investigations based on a series of experimental techniques and theoretical calculations have revealed the composition of in situ constructed CEI layers and their distribution, including the enhanced HTCN anchoring effect after lattice densification of LLOs. Finally, this study provides insights into the in situ CEI construction for enhancing the performance of high-energy and high-voltage cathode materials through effective, convenient and economical electrolyte approaches.

25 ENERGY STORAGE↗

Transferring Liquid Metal to form a Hybrid Solid Electrolyte via a Wettability-Tuning Technology for Lithium-Metal Anodes

Integrating solid-state electrolyte (SSE) into Li-metal anodes has demonstrated great promise to unleash the high energy density of rechargeable Li-metal batteries. However, fabricating a highly cyclable SSE/Li-metal anode remains a major challenge because the densification of the SSE is usually incompatible with the reactive Li metal. Here, a liquid-metal-derived hybrid solid electrolyte (HSE) is proposed, and a facile transfer technology to construct an artificial HSE on the Li metal is reported. By tuning the wettability of the transfer substrates, electron- and ion-conductive liquid metal is sandwiched between electron-insulating and ion-conductive LiF and oxides to form the HSE. The transfer technology renders the HSE continuous, dense, and uniform. The HSE, having high ion transport, electron shut-off, and mechanical strength, makes the composite anode deliver excellent cyclability for over 4000 h at 0.5 mA cm(-2) and 1 mAh cm(-2) in a symmetrical cell. When pairing with LiFePO4 and sulfur cathodes, the HSE-coated Li metal dramatically enhances the performance of full cells. Therefore, this work demonstrates that tuning the interfacial wetting properties provides an alternate approach to build a robust solid electrolyte, which enables highly efficient Li-metal anodes.

li-metal anodes↗

A New Family of Ternary Intermetallic Compounds with Dualistic Atomic Ordering – The ZIP Phases

A new family of nanostructured ternary intermetallic compounds − named the ZIP phases − is introduced in this work. The ZIP phases exhibit dualistic atomic ordering, i.e., they form two structural variants: one with the fcc diamond cubic structure (space group Fd$\bar{3}$m) and one with the hexagonal structure (space group P6 3 /mmc). They are also characterized by metallic behavior, ionic bonding, and atomic zigzagging. Powder metallurgical routes involving pressure-assisted densification are adopted to demonstrate ZIP phase synthesis in the Nb-Si-Ni, Nb-Si-Co, Ta-Si-Ni, V-Si-Ni, and Nb-Si-Fe ternary systems. Crucially, reactive hot pressing is capable of producing high-purity ZIP phase materials after the judicious, elemental system-specific optimization of the processing route. Synthesis of phase-pure materials – demonstrated in the Nb-Si-Ni ternary system by the synthesis of quasi phase-pure Nb 3 SiNi 2 and Ni 3 SiNb 2 ZIP phase-based materials – is a steppingstone to the prospective exploitation of the ZIP phases. Characterization of Nb 3 SiNi 2 and Ni 3 SiNb 2 involves crystal structure determination, spatially resolved chemical analysis, and determination of select thermal, electrical, magnetic, mechanical, and physical properties. Density functional theory is used to assess the stability of Nb 3 SiNi 2 & Ni 3 SiNb 2 and derivative binary compounds at different temperatures, also exploring the exfoliation of these two ZIP phases along specific surfaces to produce 2D derivatives.

Intermetallic compounds (IMCs)↗

3D Printed Optical Quality Silica and Silica-Titania Glasses from Sol-Gel Feedstocks

We report a method for fabricating optical quality silica and silica-titania glasses by additive manufacturing, or 3D printing. Key to this success was the combination of sol-gel derived silica and silica-titania colloidal feedstocks, 3D direct ink writing (DIW) technology, and conventional glass thermal processing methods. Printable silica and silica-titania sol inks were prepared directly from molecular precursors by a simple one-pot method, which was optimized to yield viscous, shear-thinning colloidal suspensions with tuned rheology ideal for DIW. After printing, the parts were dried and sintered under optimized thermal conditions to ensure complete organic removal and uniform densification without crystallization. Characterizations of the 3Dprinted pure silica and silica-titania glasses show that they are equivalent to commercial optical fused silica (Corning® 7980) and silica-titania glasses (Corning ULE® 7972). More specifically they exhibit comparable chemical composition, SiO2 network structure, refractive index, dispersion, optical transmission, and coefficient of thermal expansion. 3D printed silica and silica-titania glasses also exhibited comparable polished surface roughness and meet refractive index homogeneity standards within range of commercial optical grade glasses. This method establishes 3D printing as a viable tool to create optical glasses with compositional and geometric configurations that are inaccessible by conventional optical fabrication methods.

36 MATERIALS SCIENCE↗

Demonstration of the Reproducibility Challenges in the Sintering Behavior of Lithium‐Stuffed Garnets in Scaling up Synthesis

Lithium-stuffed garnets, such as Li 7 La 3 Zr 2 O 12 (LLZO), are promising candidates for next-generation solid-state batteries because of their high room-temperature ionic conductivity and chemical stability against lithium metal anodes, which are crucial for achieving higher energy density. However, realizing LLZO's potential in practical devices requires synthesis methods that can be scaled reliably to large batch sizes for manufacturing. Herein, we investigate the sintering reproducibility of LLZO synthesized at larger scales using ultrasonic spray pyrolysis, a cost-effective and scalable synthesis route. Two 100 g batches of Al-doped LLZO are prepared and their sintering behavior is examined in detail. Both Al-LLZO batches contain over 90 wt.% cubic-phase LLZO, and both batches exhibit room temperature conductivities greater than 1 × 10 −4 S cm −1 at a relative density above 0.8. However, variations in secondary phases and subtle differences in Al content lead to significant differences in densification and microstructure. These results demonstrate that LLZO's sintering behavior is highly sensitive to small changes in secondary phases and Al content, creating reproducibility challenges when moving from laboratory- to manufacturing-scale synthesis.

36 MATERIALS SCIENCE↗

Distinct Melt Infusion Architectures of Antiperovskite Solid Electrolytes

Antiperovskite solid electrolytes are an emerging class of lithium‐ion conductors distinguished by their unusually low melting points, enabling scalable, low‐temperature processing routes not accessible to most solid electrolytes. In this work, we synthesize phase‐pure chloride (Cl), bromide (Br), and mixed halide (ClBr) variants of antiperovskites and investigate their ionic conductivities in both powder and hot‐pressed forms. Hot pressing significantly enhances conductivity across all compositions, while energy‐dispersive X‐ray spectroscopy (EDS) of the mixed halide system reveals halide surface migration during densification. We further investigate the melt‐infiltration behavior of these electrolytes into substrates relevant to solid‐state battery architectures, including Al and Cu current collectors, conventional NMC and LFP cathodes, and a foamed NMC cathode with a highly porous architecture. The foamed cathode enables deep and uniform electrolyte penetration, highlighting the role of electrode architecture in facilitating melt infiltration. Across all substrates, electrolyte halide chemistry strongly influences wetting behavior, penetration depth, and resulting microstructural morphology. Together, these results establish clear processing–structure relationships for melt‐infiltrated antiperovskite solid electrolytes and demonstrate how electrolyte chemistry and electrode architecture govern interfacial morphology during integration, providing practical guidelines for processing and structural design in solid‐state battery systems.

antiperovskite↗

A spatially distributed model for assessment of the effects of changing land use and climate on urban stream quality: Development of a Spatially Distributed Urban Water Quality Model

While the effects of land use change in urban areas have been widely examined, the combined effects of climate and land use change on the quality of urban and urbanizing streams have received much less attention. We describe a modeling framework that is applicable to the evaluation of potential changes in urban water quality and associated hydrologic changes in response to ongoing climate and landscape alteration. The grid-based spatially distributed model, DHSVM-WQ, is an outgrowth of the Distributed Hydrology-Soil-Vegetation Model (DHSVM) that incorporates modules for assessing hydrology and water quality in urbanized watersheds at a high spatial and temporal resolution. DHSVM-WQ simulates surface runoff quality and in-stream processes that control the transport of nonpoint-source (NPS) pollutants into urban streams. We configure DHSVM-WQ for three partially urbanized catchments in the Puget Sound region to evaluate the water quality responses to current conditions and projected changes in climate and/or land use over the next century. Here we focus on total suspended solids (TSS) and total phosphorus (TP) from nonpoint sources (runoff), as well as stream temperature. The projection of future land use is characterized by a combination of densification in existing urban or partially urban areas, and expansion of the urban footprint. The climate change scenarios consist of individual and concurrent changes in temperature and precipitation. Future precipitation is projected to increase in winter and decrease in summer, while future temperature is projected to increase throughout the year. Our results show that urbanization has a much greater effect than climate change on both the magnitude and seasonal variability of streamflow, TSS and TP loads largely due to substantially increased streamflow, and particularly winter flow peaks. Water temperature is more sensitive to climate warming scenarios than to urbanization and precipitation changes. Future urbanization and climate change together are predicted to significantly increase annual mean streamflow (up to 55%), water temperature (up to 1.9 ºC), TSS load (up to 182%), and TP load (up to 74%).

Sun, Ning↗

Quantifying the cooperative evolution of microphase segregation and nanostructural order in annealed polyurethanes of MDI-BDO-PTHF

Here, we quantify the relationship between microphase segregation and local structure development in thermoplastic polyurethanes. Samples were prepared with varying ratios of 4,40 -methylene diphenyl diisocyanate (MDI) and 1,4-butanediol (BDO) to polytetrahydrofuran (PTHF) and annealed at temperatures T a between RT–140 °C for 20 h each. Distinct populations of smaller and larger ordered domains are distinguished by pair distribution func tion analysis. The intermediate-range order of nanoscale hard domains in the paracrystalline state (form I) is directly extracted and characterized. The results suggest that form I of the MDI-BDO:PTHF system presents a conformational and packing order similar to the form III structure, typically obtained from stretching/annealing, but with limited spatial coherence of 3–7 nm. Heating above T g of the hard segments is necessary to achieve a substantial structural response from the annealing treatment. Increasing T a promotes purification of the soft phase via microphase segregation, coalescence of the hard blocks, and growth of paracrystalline phase, while a minority fraction of longer-range ordered domains left over from production remains relatively constant. We observe a composition-dependent decrease in the average nearest-neighbor dis tance that can be correlated with the greater number of C C, C N, and C O bonds with increased hard segment content. A non-linear deviation in the trend is observed to correlate with sample densification. The mechanical and thermal behavior of the samples is intimately tied to the segregation state.

processing-structure-properties↗