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At least 217 records · Page 12

Effect of gravity on liquid phase sintering

The unique conditions offered by the earth orbital environment in material processing involving both solid and liquid phases, such as liquid phase sintering, were studied. An experimental development program involving both test and theoretical work was initiated. Experimental work using material combinations selected such that maximum information about the effect of gravity can be derived has been conducted. Wetting of the solid phase by the liquid during sintering is an important phenomenon in liquid phase sintering, and gravity has influence on both capillary phenomenon and density segregation; hence, material combinations were selected such that these two effects can be suitably studies. The experimental work is meant to form the basis for similar comparative work done under low-g conditions. The part of the model dealing with the capillary phenomenon, as related to liquid phase sintering and the effect of gravity on it, suggest that gravity will have negligible effect on the Bond number and that the cohesive force is dependent on both the amount of liquid phase and the angle of contact.

Mookherji, T.↗

Pressureless sintering of lithium hydride

Lithium Hydride is a material of growing importance for addressing technological challenges related to nuclear fusion, long-term human space travel, and thermal energy storage. Pressureless sintering provides a straightforward, scalable approach to produce dense LiH parts of all sizes and shapes. Pressed LiH green compacts were sintered at heating rates from 2.5 to 20 °C/min to 650 °C, yielding densities up to 96 ± 1.4 %, with densification initiating at 500 °C. Here, a validated master sintering curve was constructed with a sintering apparent activation energy of 135 kJ/mol. X-ray diffraction and simultaneous thermal analysis revealed Li 2 O formation from 300 – 550 °C and decomposition of LiH into Li metal at 550 °C, each reflected as deviations in the master sintering curve. Computed tomography after thermal treatment to 550 °C showed the formation of corrosion products, and after thermal treatment to 650 °C LiH reduction to Li most significantly at exposed surfaces.

36 MATERIALS SCIENCE↗

Metal Fused Filament Fabrication of Titanium Alloy for In Space Manufacturing

NASA is developing materials and processes for the in-space manufacturing of many items for the International Space Station (ISS) and future exploration platforms. These new manufacturing processes will require the further development of current 3D printing processes to achieve high-performance metal parts within the power and space constraints of the ISS. Manufacturing Ti-6Al-4V alloy parts with 3D printing using a metal fused filament fabrication (MF3) process is an alternative process to the Direct Metal Laser Sintering (DMLS) of the metal powders additive manufacturing process. Our initial work fabricating Ti-6Al-4V parts from Ti-6Al-4V powder-binder feedstock and processed with the MF3 process has resulted in 95-97% sintered densities. The current development work of optimized sintered properties investigates the effects of variation in sintering time, temperature, and vacuum on the sintered properties of Ti-6Al-4V MF3 printed tensile bars. Sintered properties such as density, hardness, and tensile properties were characterized followed by microstructural and chemical (O/C/N) analysis to understand the role of sintering process on the ensuing material properties. Future development of the MF3 process will also involve investigation of the effects of micro-milling the Ti-64Al-4V powder to nanometer particle sizes and the investigation of laser sintering of the 3D printed devices. This new micro-milling technique will have broad application to other areas that require particle size reduction of hard metallic materials, such as Nuclear Thermal Propulsion and other NASA technologies. Laser sintering in lieu of high temperature thermal sintering should allow for significant power reduction and improved processing speeds.

sintering, alloys, 3D printing↗

Preparation Of Sources For Plasma Vapor Deposition

Multicomponent metal targets serving as sources of vapor for plasma vapor deposition made in modified pressureless-sintering process. By use of targets made in modified process, one coats components with materials previously plasma-sprayed or sintered but not plasma-vapor-deposited.

Waters, William J.↗

Fabrication of highly dense SiN4 ceramics without additives by high pressure sintering

Silicon nitride (Si3N4) is one of candidate materials for the engineering ceramics which is used at high temperatures. The mechanical strengths of hot pressed or sintered Si2N4 ceramics containing some amount of additives, however, are deteriorated at elevated temperatures. To improve the high temperature strength of Si3N4 ceramics, an attempt to consolidate Si3N4 without additives was made by high pressure sintering technique. Scanning electron micrographs of fracture surfaces of the sintered bodies showed the bodies had finely grained and fully self-bonded sintered bodies were 310N sq m at room temperature and 174N/sq m at 1200 C.

Takatori, K.↗

Reflectance Spectra Diversity of Silica-Rich Materials: Sensitivity to Environment and Implications for Detections on Mars

Hydrated silica-rich materials have recently been discovered on the surface of Mars by the Mars Exploration Rover (MER) Spirit, the Mars Reconnaissance Orbiter (MRO) Compact Reconnaissance Imaging Spectrometer for Mars (CRISM), and the Mars Express Observatoire pour la Mineralogie, l'Eau, les Glaces, et l'Activite'(OMEGA) in several locations. Having been interpreted as hydrothermal deposits and aqueous alteration products, these materials have important implications for the history of water on the martian surface. Spectral detections of these materials in visible to near infrared (Vis NIR) wavelengths have been based on a H2O absorption feature in the 934-1009 nm region seen with Spirit s Pancam instrument, and on SiOH absorption features in the 2.21-2.26 micron range seen with CRISM. Our work aims to determine how the spectral reflectance properties of silica-rich materials in Vis NIR wavelengths vary as a function of environmental conditions and formation. Here we present laboratory reflectance spectra of a diverse suite of silica-rich materials (chert, opal, quartz, natural sinters and synthetic silica) under a range of grain sizes and temperature, pressure, and humidity conditions. We find that the H2O content and form of H2O/OH present in silica-rich materials can have significant effects on their Vis NIR spectra. Our main findings are that the position of the approx.1.4 microns OH feature and the symmetry of the approx.1.9 microns feature can be used to discern between various forms of silica-rich materials, and that the ratio of the approx.2.2 microns (SiOH) and approx.1.9 microns (H2O) band depths can aid in distinguishing between silica phases (opal-A vs. opal-CT) and formation conditions (low vs. high temperature). In a case study of hydrated silica outcrops in Valles Marineris, we show that careful application of a modified version of these spectral parameters to orbital near-infrared spectra (e.g., from CRISM and OMEGA) can aid in characterizing the compositional diversity of silica-bearing deposits on Mars. We also discuss how these results can aid in the interpretation of silica detections on Mars made by the MER Panoramic Camera (Pancam) and Mars Science Laboratory (MSL) Mast-mounted Camera (Mastcam) instruments.

Rice, M. S.↗

Moon to Mars Planetary Autonomous Construction Technology (MMPACT) Lunar Surface Construction Activity at NASA Marshall Space Flight Center

Introduction: The goal of the Moon to Mars Planetary Autonomous Construction Technology (MMPACT) Project at NASA Marshall Space Flight Center (MSFC) is to develop, deliver, and demonstrate on-demand capabilities to protect astronauts and create infrastructure elements on the lunar surface via construction of landing pads, habitats, shelters, roadways, berms, and blast shields using lunar regolith-based materials. MSFC has strong collaborations with industry, academia, and other NASA Centers to accomplish this goal. The MMPACT project consists of three elements. The first focuses on the development of an autonomous construction system. The second focuses on construction feedstock materials development. The third element focuses on the development of a microwave sintering construction capability. The team plans to demonstrate construction on a small Commercial Lunar Payload Services (CLPS) lander in the 2025 timeframe, with a future goal of constructing a subscale landing pad in 2028-2029.The MMPACT project is funded through the Lunar Surface Innovation Initiative, which is part of the Space Technology Mission Directorate. Technology Development: The MMPACT team will evaluate multiple autonomous construction and microwave construction technologies, materials, and construction element forms. Selected technologies will be matured; processes and operations will be defined for the two flight missions. Evaluations of materials, as well as the technology itself, will be demonstrated in simulated lunar environments as part of the technology maturation process. The team is keenly aware of the properties of the lunar environment. Its temperature swings, negligible exosphere, and unprepared site foundations factor into the materials for both construction and hardware, the concept of operations, and the technology’s interdependencies. Materials: The team is looking at materials that can be produced from in-situ resources in an effort to make lunar construction cost-effective. The particular focus of the materials team is cementitious materials, metals, and sintered and melted regolith. These materials will be studied for tensile, compressive, and flexural strength. They will also be tested for their ability to handle thermal swings and vacuum. They will be fully characterized using various microscopy techniques to examine micro-structures, chemistry, and crystal formation. Interdependencies: There are many interdependencies that MMPACT has already identified. These include: •Excavation interface •Regolith feedstock beneficiation •Regolith feedstock storage and provision •Requirements for structures •Site-to-site mobility systems •Availability of lunar simulant •Lander off-loading capabilities •Navigation systems •Power •Regolith composition and mineralogy •Lander specifications •Communication protocols Technology developments in these additional areas would be beneficial to MMPACT.

Moon to Mars Planetary Autonomous Construction Tec↗

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.

20 FOSSIL-FUELED POWER PLANTS↗

Testing of spark plasma sintered porous tungsten under neon glow discharge cleaning conditions in LTX-β

This paper demonstrates that tungsten (W) based powder reconstituted Plasma Facing Components (PFCs) can be treated in situ in a fusion reactor to remove W oxide and carbon (C) contamination. Doing so should ease the challenge of using these materials in a Capillary Porous System (CPS) with lithium (Li) by enabling better wetting and less contamination of the Li by the underlying CPS. Most powder reconstituted materials including 3D printed and sintered PFCs suffer from a high surface contamination from oxides and surface C, which complicates their use with liquid Li, a primary PFC candidate. Spark plasma sintered porous W samples were fabricated to be used as a CPS with liquid Li. The samples were characterized in terms of morphology and surface chemistry. Analysis confirms a high C and oxygen (O) contamination. We present the results of exposing this type of CPS to Glow Discharge Cleaning (GDC) cycles in the Lithium Tokamak Experiment-β (LTX-β). The sample was exposed to neon (Ne) GDC in the midplane of the low-field side of LTX-β and analyzed in vacuo with Temperature Programmed Desorption (TPD) and Secondary Ion Mass Spectrometry (SIMS) to investigate the effects the Ne GDC had on the chemical composition of the sample. The combination of Ne GDC with rapid heating as done in TPD was successful in reducing the W oxides and removing the C contamination.

Capillary porous system↗

Zirconium-diboride silicon-carbide composites: A review

Zirconium diboride (ZrB 2 ) and silicon carbide (SiC) composites have long been of interest since it was observed that ZrB 2 improved the thermal shock resistance of SiC. However, processing of these materials can be difficult due to high and different sintering temperatures and differences in the thermodynamic stability of each material. ZrB 2 –SiC composites have been processed in a variety of ways including hot-pressing, spark-plasma sintering, reactive melt infiltration, pack cementation, chemical vapor deposition, chemical vapor infiltration, stereolithography, direct ink writing, selective laser sintering, electron beam melting, and binder jet additive manufacturing. Each manufacturing method has its own pros and cons. This review serves to summarize more than 60 years of research and provide a coherent resource for the variety of methods and advancements in development of ZrB 2 –SiC composites.

36 MATERIALS SCIENCE↗

Electrically conductive proppant

Electrically conductive sintered, substantially round and spherical particles and methods for producing such electrically conductive sintered, substantially round and spherical particles from an alumina-containing raw material. Methods for using such electrically conductive sintered, substantially round and spherical particles in hydraulic fracturing operations.

Cannan, Chad↗

Unraveling the nature of sulfide ions in hydrometallurgical recycling of NCM622 cathode material

The use of lithium-ion batteries (LIBs) has increased dramatically since its initial inception in the late 20th century. Such a surge in the LIB market and industry has resulted in a huge demand for mineral resources. Besides, the large scale of production will lead to massive amounts of waste batteries in the end. As such, recycling is seen as an end-of-pipe process to resolve sustainability and environmental concerns. The hydrometallurgical recycling is considered to be the most prominent method to recover cathode materials from spent LIBs owing to its high leaching efficiency and low energy costs. A series of procedures including pretreatment of the spent LIBs, acid leaching of the black mass, chemical co-precipitation of the hydroxide precursor, and sintering of the cathode active material need to be operated precisely. In this aspect, the impurities introduced during the process could pose a serious threat to the reaction stability as well as recycling consistency. Here, the impact of sulfide ions on recovered LiNi 0.6 Co 0.2 Mn 0.2 O 2 (NCM622) cathode material with the method of hydrometallurgy is first investigated in detail. This study shows that hydrometallurgical process is not obviously influenced by sulfide impurity. No signs of secondary phase or impurity inclusion are spotted in synthesized cathodes. Under 5 at % sulfide concentration conditions, the obtained NCM622 cathode exhibits a capacity of 159.4 mAh/g after 100 cycles at 1/3C, which is at the same level as virgin benchmark. The difference in rate performance between cathodes with and without additional sulfide is less than 2 % or even smaller. In short, the results indicate a neutral status of sulfide ions in hydrometallurgical recycling.

25 ENERGY STORAGE↗

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↗

The sol–gel autocombustion as a route towards highly CO 2 -selective, active and long-term stable Cu/ZrO 2 methanol steam reforming catalysts

The adaption of the sol-gel autocombustion method to the Cu/ZrO 2 system opens new pathways for the specific optimisation of the activity, long-term stability and CO 2 selectivity of methanol steam reforming (MSR) catalysts. Calcination of the same post-combustion precursor at 400 °C, 600 °C or 800 °C allows accessing Cu/ZrO 2 interfaces of metallic Cu with either amorphous, tetragonal or monoclinic ZrO 2 , influencing the CO 2 selectivity and the MSR activity distinctly different. While the CO 2 selectivity is less affected, the impact of the post-combustion calcination temperature on the Cu and ZrO 2 catalyst morphology is more pronounced. A porous and largely amorphous ZrO 2 structure in the sample, characteristic for sol-gel autocombustion processes, is obtained at 400 °C. This directly translates into superior activity and long-term stability in MSR compared to Cu/tetragonal ZrO 2 and Cu/monoclinic ZrO 2 obtained by calcination at 600 °C and 800 °C. The morphology of the latter Cu/ZrO 2 catalysts consists of much larger, agglomerated and non-porous crystalline particles. Based on aberration-corrected electron microscopy, we attribute the beneficial catalytic properties of the Cu/amorphous ZrO 2 material partially to the enhanced sintering resistance of copper particles provided by the porous support morphology.

36 MATERIALS SCIENCE↗

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.↗

The effects of surface finish and grain size on the strength of sintered silicon carbide

The effects of surface treatment and microstructure, especially abnormal grain growth, on the strength of sintered SiC were studied. The surfaces of sintered SiC were treated with 400, 800 and 1200 grit diamond wheels. Grain growth was induced by increasing the sintering times at 2050 C. The beta to alpha transformation occurred during the sintering of beta-phase starting materials and was often accompanied by abnormal grain growth. The overall strength distributions were established using Weibull statistics. The strength of the sintered SiC is limited by extrinsic surface flaws in normal-sintered specimens. The finer the surface finish and grain size, the higher the strength. But the strength of abnormal sintering specimens is limited by the abnormally grown large tabular grains. The Weibull modulus increases with decreasing grain size and decreasing grit size for grinding.

You, Y. H.↗

Permeability of Candidate Stirling Heater Head Materials Measured

Researchers at the NASA Glenn Research Center are evaluating high-temperature materials for Stirling heater heads for second- and third-generation Stirling radioisotope power systems that would help to increase the system efficiency to 30 to 35 percent and the system specific power to 8 to 10+ W/kg. Ceramic materials could make it possible for the convertor hot-end temperature to be increased to 1050 to 1200 C, in comparison to the current 650 C with an Inconel 718 heater head. A hermetically sealed Stirling heater head must retain a constant internal pressure of nearly 400-psi helium (He) throughout its useful life (120,000 hr) at the design operating temperature. Therefore, He permeability was measured for eight potential materials and compared with the permeability of the current heater head material, Inconel 718. The eight materials included silicon nitride (Si3N4), silicon dioxide (SiO2), both sintered and chemical vapor deposited (CVD) silicon carbide (SiC), alumina (Al2O3), two types of melt-infiltrated (MI) SiC/SiC composites, and a carbon/SiC composite (C/SiC). Glenn submitted samples of each material to Porous Materials, Inc., Ithaca, New York, for permeability analysis. At room temperature and 30-psi He, four materials--Si3N4, Al2O3, SiO2, and sintered SiC--demonstrated lower permeability than Inconel 718. The CVD SiC and all the composite materials were significantly more permeable to He than the baseline material.

Freedman, Marc R.↗

Development of large-scale, 3D Printed high temperature ceramic material

Through this collaborative effort, a new 3D printing platform for ceramics called laser-induced slip casting (LIS) was explored and developed for improving the processing and manufacture of silicon carbide (SiC), a high temperature ceramic material. This method prints layers of ceramic slips/slurries with subsequent selective-laser heating to dry each layer to build a 3D structure. The completed and dried part is then sintered. This manufacturing process is inherently lower cost than alternative ceramic printing methods such as binder jet technology or stereolithography when it comes to the feedstock material but is more expensive than robocasting or direct ink writing. However, it has the potential to make more controlled parts with less defects compared to robocasting. The largest cost is the heating source for the printer. With this technique, there is potential to make large ceramic parts in a near-net shape. Further, there is no known commercial manufacturing of 3D printed ceramics that creates a large range of different high-density ceramics at large scale. The goals and outcomes for the development of the new printing technology were: 1) assessing the technology with alumina by characterizing coupons, 2) printing and sintering of silicon carbide (SiC), and 3) characterization and properties testing of materials printed and a scale-up of SiC part(s). Through this collaborative project, it was sought to provide the best solution to achieving highly dense and near-net shaped ceramic parts at large scale and reduced cost. The goal was to produce high density sintered materials for applications in defense, energy generating systems, armor, and wear parts using 3D printing methods. Variables including powder particle sizes, dispersant molecular weights (MWs), binders, printing parameters, and post processing were explored as well as the characterization of the physical properties (add specifics here).

36 MATERIALS SCIENCE↗