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At least 127 records · Page 7

All sources NASA NTRS DOE OSTI

NASA NTRS1980

Sintered reaction bonded Si3N4 for the AGT 101 turbine rotor

The sintered reaction reaction bonded Si3N4 (SRBSN) process, with Y2O3 as a sintering aid, was selected for the fabrication of the AGT 101 turbine rotor. Experiments to determine the optimum Y2O3 composition of this system are discussed. The room temperature strength of the optimum material (RM-1) exceeds 700 MPa while the 1200 C strength exceeds 550 MPa. The slip casting fabrication technique employed for the AGT 101 simulated rotor is described. Rotors have been cast, nitrided and sintered. Densities exceeding 97% of theoretical (3.26 g/cc) have been obtained. Problems relating to sintering reproducibility, and the overall quality of the simulated rotors have been identified.

Mangels, J. A.↗

NASA NTRS1982

Microstructure and property characterization of sintered Si3N4, SiC, and SiAlON

Commercially-produced, pressureless sintered Si3N4, SiC, and SiAlON were characterized with respect to density, phases present, bend strength, and oxidation resistance. The room-temperature bend strengths of sintered Si3N4, SiC, and SiAlON are comparable. However, the room-temperature strengths are much lower (approximately 40 to 50%) than the room-temperature strength of hot-pressed Si3N4 (NC-132). The strength loss in Si3N4 and SiAlON materials at high temperature was attributed to a viscous grain-boundary phase, retained during cooling from the sintering temperature. The oxidation resistance of sintered alpha-SiC was the best of any materials tested.

Dutta, S.↗

NASA NTRS1983

Sintering, properties and fabrication of Si3N4 + Y2O3 based ceramics

Pure silicon nitride shows a remarkable resistance to sintering without the use of densification additives. The present investigation is concerned with results which show the effect of chemical content on sinterability, taking into account the composition, raw material impurities, and processing contaminants. Aspects of sintering are discussed along with strength characteristics, and oxidation relations. Attention is given to phase field I and II materials, phase field III and IV materials, tungsten carbide and oxidation at 600 C, and studies involving shape fabrication by injection molding. It was found that in sintering Si3N4 + Y2O3 an increase in the amount of Y2O3 and, in particular, the addition of Al2O3 enhances the fluidity of the liquid phase.

Quackenbush, C. L.↗

NASA NTRS1985

Sintered Lining for Heat-Pipe Evaporator

Hotspots eliminated by lining inner wall. Distribution of heat transfer liquid in heat-pipe evaporator improved by lining inner wall with layer of sintered metal. Sintered layer takes place of layer of screen wick formerly sintered or bonded to wall. Since sintered layer always full of liquid, no hotspot of type that previously arose where former screen wick did not fit properly against wall.

Ernst, D. M.↗

NASA NTRS1984

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.↗

NASA NTRS1985

Manufacture of dense sintered bodies containing silicon nitride

Sintered bodies containing 1-32.5 Si oxide and 1.5 wt.% SiC (Si oxide/SiC wt. ratio 3/2) are prepared and kept in a 10-3000 kg/2 sq. cm. N (g) atmosphere at 1500-2300 degrees, while simultaneously maintaining the CO (g) partial pressure around the body lower than the nitrogenation equil. pressure to give a dense sintered body. The prepared dense sintered body has high strength at high temperatures. Thus, SiC 40, oxide 30 and Si3N4 30 wt% were fired to a body which was kept in 1500 kg/sq. cm. N (g) for 20 h at 2000 degrees to give a dense sintered body having high bending strength at high temperatures.

Hirota, K.↗

NASA NTRS1986

On the sintering of silicon carbide

This document deals with the sintering of silicon carbide using pressureless sintering. This technique makes it possible to sinter a primarily covalent material to usable densities up to over 98% thD without having to use a high amount of sinter additives as is the case with other non-oxide ceramic materials. The process takes place rapidly, and it is also possible to produce relatively thick-walled structural parts without major problems. This sheds more light on the true characteristics of silicon carbide in one structural part, since there is no second or nearly no second phase. Heat pressing has improved stability.

Gugel, E.↗

NASA NTRS1989

Strength of hot isostatically pressed and sintered reaction bonded silicon nitrides containing Y2O3

The hot isostatic pressing of reaction bonded Si3N4 containing Y2O3 produced specimens with greater room temperature strengths than those by high pressure nitrogen sintering of the same material. Average room temperature bend strengths for hot isostatically pressed reaction bonded silicon nitride and high pressure nitrogen sintered reaction bonded silicon nitride were 767 and 670 MPa, respectively. Values of 472 and 495 MPa were observed at 1370 C. For specimens of similar but lower Y2O3 content produced from Si3N4 powder using the same high pressure nitrogen sintering conditions, the room temperature strength was 664 MPa and the 1370 C strength was 402 MPa. The greater strengths of the reaction bonded silicon nitride materials in comparison to the sintered silicon nitride powder material are attributed to the combined effect of processing method and higher Y2O3 content.

William A Sanders↗

NASA NTRS1989

Ultrasonic imaging of porosity variations produced during sintering

A silicon carbide disk was sintered from 2090 to 2190 C in 25-C steps. After each sintering step, the disk was examined using a precision acoustic scanning system to determine acoustic attenuation and velocity. The bulk density was found to vary nonmonotonically with sintering temperature. The density varied as much as 10 percent from its value at 2090 C during the sintering process. Local density fluctuations occurred in an organized and history-dependent way. These local density fluctuations varied up to + or - 7 percent of the bulk density and were made visible by acoustic attenuation and velocity mapping.

Generazio, Edward R.↗

NASA NTRS1992

Laboratory studies on cometary crust formation: The importance of sintering

It is demonstrated by experiments and theoretical considerations that sintering processes, so far used to describe the densification of metal and ceramic powders, are relevant for icy materials and therefore probably also for comets. A theoretical model is presented which describes the evolution of so called sinter necks, the contact zone between ice particles. With this model the strength increase of a porous, loosley packed icy body is calculated in which the sinter necks grow by evaporation and condensation of water vapor at a constant temperature. Experiments with ice powders validate the model qualitatively. An increase in strength up to a factor of four is observed during isothermal sintering. In order to check the relevance of the experimental results and the basic theoretical ideas with respect to real comets, more exact theories and improved experiments taking into account additional mass transport mechanisms are needed.

Ratke, L.↗

NASA NTRS1954

Permeability and Strength Measurements on Sintered, Porous, Hollow Turbine Blades Made by the American Electro Metal Corporation under Office of Naval Research Contract N-ONR-295 (01)

An experimental investigation was made to determine the permeability and strength characteristics of a number of sintered, porous, hollow turbine rotor blades and to determine the effectiveness of the blade fabrication method on permeability control. The test blades were fabricated by the American Electro Metal Corporation under a contract with the Office of Naval Research, Department of the Navy, and were submitted to the NACA for testing. Of the 22 test blades submitted, ten were sintered but not coined, five were sintered and coined, and seven were sintered and not coined but contained perforated reinforcements integral with the blade shells. Representative samples of each group of blades were tested. Large variations in permeability in both chordwise and spanwise directions were found. Local deviations as large as 155 to -85 percent from prescribed values were found in chordwise permeability. Only one blade, an uncoined one, had a chordwise permeability variations which reasonably approached that specified. Even for this blade, local deviations exceeded 10 percent. Spanwise permeability, specified to be held constant, varied as much as 50 percent from root to tip for both an uncoined and a coined blade. Previous NACA analyses have shown that in order to maintain proper control of blade wall temperatures, permeability variations must not exceed plus or minus 10 percent. Satisfactory control of permeability in either the chordwise or the spanwise direction was not achieved in the blades tested. Spin tests made at room temperature for six blades revealed the highest material rupture strength to be 8926 pounds per square inch. This value is about one third the strength required for rotor blades in present-day turbojet engines. The lowest value of blade strength was 1436 pounds per square inch.

Richards, Hadley T.↗

NASA NTRS2011

Implementation Challenges for Sintered Silicon Carbide Fiber Bonded Ceramic Materials for High Temperature Applications

During the last decades, a number of fiber reinforced ceramic composites have been developed and tested for various aerospace and ground based applications. However, a number of challenges still remain slowing the wide scale implementation of these materials. In addition to continuous fiber reinforced composites, other innovative materials have been developed including the fibrous monoliths and sintered fiber bonded ceramics. The sintered silicon carbide fiber bonded ceramics have been fabricated by the hot pressing and sintering of silicon carbide fibers. However, in this system reliable property database as well as various issues related to thermomechanical performance, integration, and fabrication of large and complex shape components has yet to be addressed. In this presentation, thermomechanical properties of sintered silicon carbide fiber bonded ceramics (as fabricated and joined) will be presented. In addition, critical need for manufacturing and integration technologies in successful implementation of these materials will be discussed.

Singh, M.↗

DOE OSTI2024

Spark plasma sintering of fuel meats for U 3 O 8 based dispersion fuels

Research and test reactors often use dispersion-type fuel due to its increased thermal conductivity and burn-up capabilities compared to conventional fuel. Al-U 3 O 8 (aluminumtriuranium octaoxide) dispersion fuels have several advantages over their competitors, such as higher service temperature and better stability of oxygen stoichiometry. However, the two-step fabrication of dispersion fuel causes undesirable porosity in cold-pressed fuel meats that is preserved in co-extruded fuel plates. To combat this, spark plasma sintering (SPS) was used for the fabrication of Al-15, 20, and 30 vol% U 3 O 8 and 8 and 12 vol% Mo-U 3 O 8 fuel meats for the Al-U 3 O 8 time. The in situ SPS data was used to construct and validate Master Sintering Curves (MSCs) with accuracies in Al fuels at 0.02 g/cm 3 , and Mo fuels at 0.07 and 0.17 g/cm 3 . The as-sintered fuel meats were characterised using x-ray diffraction (XRD) and scanning electron microscopy (SEM) to understand chemical and physical changes following the SPS process. The pellets exhibited very high relative densities, the U 3 O 8 was observed to undergo reduction to UO 2 .

Aluminium↗

DOE OSTI2025

Induction ultrafast sintering

This study proposes and demonstrates induction ultrafast sintering (IUS), which enables rapid densification of refractory and other materials via two contactless modalities: direct IUS (d-IUS), where heating occurs through electromagnetic coupling with the sample, and susceptor IUS (s-IUS), where heating is achieved indirectly via an induction-heated metal case. Ultrahigh heating rates of ∼75 to >450 °C/s and temperatures exceeding 2500 °C are readily achieved. Both d-IUS and s-IUS densify molybdenum to high densities within 120 s, with only ∼1–3 % porosity observed by image analysis. Similarly, 3 mol % yttria-stabilized zirconia (3YSZ) reaches ∼97 % relative density in 30 s via s-IUS. This study further demonstrates ultrafast reactive sintering of two difficult-to-sinter materials: a refractory compositionally complex alloy–carbide (RCCA–CCC) composite, NbMoTaW–(Nb 0.37 Mo 0.11 Ta 0.39 W 0.13 ) 2 C, using d-IUS, and a compositionally complex silicide (CCS), (Mo 1/3 Nb 1/3 Zr 1/3 )Si 2 , using s-IUS. This IUS platform offers a versatile route for high-throughput materials discovery and energy-efficient fabrication of bulk refractory materials.

36 MATERIALS SCIENCE↗

DOE OSTI2025

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↗

DOE OSTI2023

In situ probing of interfacial roughness and transient phases during ceramic cold sintering process

The ceramic cold sintering process (CSP) offers an eco-friendly approach to producing fully dense ceramics at low temperatures. However, an incomplete mechanistic understanding hinders its optimization and widespread adoption. In this study, we analyze the microstructural and structural changes in ZnO, a model CSP system, using in situ synchrotron-based high-energy small-angle X-ray scattering and X-ray diffraction techniques. Our results reveal the time evolution of ZnO particles' surface area and roughness, reflecting the dissolution and re precipitation processes that enable densification. The in situ measurements supply valuable kinetic data for these stages of CSP. Alongside microstructural changes and densification, we observed the evolution of secondary phases representing reaction products between ZnO and acetic acid, the solvent used. The initial ZnO/solvent mixture's dominant secondary phase is attributed to zinc acetate, which is gradually replaced by a zinc soap-type structure during CSP. This structure has a large (≈ 21 Å) lattice parameter and is assumed to have a layered nature. The formation of this soap phase, which is retained in the sintered product as an intergranular component, appears to be a signature of successful cold sintering as it facilitates mass transport, leading to densification. Here, our study underscores the potential of in situ synchrotron characterization for revealing microstructural and phase-evolution details during CSP. These findings, which would be challenging to obtain through ex situ measurements, provide crucial data to guide and validate theoretical models, ultimately enhancing CSP's effectiveness and adoption.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Electrochemical grand potential-based phase-field simulation of electric field-assisted sintering

Here, an electrochemical grand potential functional was proposed to describe the sintering of an ionic ceramic green body. The resultant phase-field description enables simulation of the consolidation of an arbitrary number of granular particles and their interactions with the surrounding void phase. The model includes the effects of charged vacancies and the associated interactions between internal and applied electric fields. Defect segregation to grain boundaries is also accounted for, as well as enhanced interfacial defect mobilities. The model was parameterized for Y 2 O 3 . Simulations of two-particle systems showed that the applied electric field had an increasingly important impact on neck growth as particle size increased. A sudden rapid increase in temperature occurred for larger field strengths, which has been reported to be correlated to the onset of a flash event in flash sintering. Simulations of many particles showed that internal heat generation by Joule heating was localized at particle–particle contacts (grain boundaries), even though their conductivities were lower than nearby internal particle-void interfaces. A percolative path for ionic charge across the green body and the ceramic sintered solid was thus defined, accelerating the Joule heating process as the porosity of the green body is removed.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Mechanically strengthened heterogeneous Sm-Co sintered magnets

Samarium-cobalt sintered magnets offer excellent magnetic properties, thermal stability, and corrosion resistance. They are used in a variety of defense and civilian applications, especially when elevated operation temperatures (e.g., 200 ºC to 550 ºC) are required. However, the utilization of these materials is restricted by their brittleness. Improving their mechanical resilience would make them more cost-effective, efficient, and robust in decarbonization and other function-related applications while reducing the pressure on critical material supply chains. In this paper, we engineer a series of novel heterogeneous microstructures, such as laminated coarse grain (CG)/fine grain (FG) and core/shell CG/FG microstructures, to produce unprecedented combinations of superior mechanical and magnetic properties without altering the chemical compositions of the magnets or common heat treatment procedures. Further, a 60% flexural strength enhancement is obtained using heterogeneous Sm 2 (CoFeCuZr) 17 sintered magnets with little impact on their magnetic properties. The mechanically robust heterogeneous Sm-Co sintered magnets have a minor (e.g., less than 4.6%) reduction in the energy product (BH) max due to a slightly reduced squareness of the demagnetization curve, with no decrease in either the remanence (B r ) or the intrinsic coercivity (H ci ). The flexural strengths of these heterogeneous Sm-Co magnets depend on the volume ratios and mean grain sizes of the FG/CG regions, as well as their microstructural architectures. The fine-grained regions act as mechanical strengthening sites, which can be strategically used when designing the magnet for different applications. This technology is highly compatible with existing magnet manufacturing processes and thus can be adopted readily by the magnet industry.

36 MATERIALS SCIENCE↗