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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 271 records · Page 15
All sourcesNASA NTRSDOE OSTI
DOE OSTI2020

Optimization of Lithium Content and Sintering Additives in Tape Cast Lithium Garnet Electrolyte Sheets

The lithium garnet (LLZO) remains one of the most promising electrolyte materials for producing solid state batteries. Tape casting is one method for producing the thin ceramic electrolyte layer required for a high-performance solid state battery. Processing of LLZO is complicated by several factors including lithium volatilization, abnormal grain growth and phase instability. Many of these issues are exacerbated in tape cast sheets by the sheets' higher surface area to volume ratio, when compared to pellet processing methods. Here, we report on an environmentally friendly aqueous tape casting process for LLZO using methylcellulose as a binder and compare final sheet properties to other, solvent-based, options. Solids loading, binder content, dispersant composition, and wetting agent type are varied to improve ease of casting and enhance properties of the as-cast tape. Lithium content in sintered LLZO sheets is controlled by the inclusion of excess Li 2 CO 3 as lithium source in the ceramic tape itself and by a novel method of producing a lithium-saturated furnace atmosphere. Sintering time and temperature are optimized, and rapid thermal processing is investigated as a method of reducing lithium loss. Al 2 O 3 and MgO are examined for use as sintering additives. Characterization of LLZO sheets is performed with XRD, EIS and SEM. Li 2 CO 3 and sintering additive levels are optimized for ionic conductivity and density. The optimization effort improved the conductivity and density of 100µm thick sintered sheets to greater than 3x10 -4 S/cm conductivity and 90% density.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Development of an Innovative High-Thermal Conductivity UO2 Ceramic Composites Fuel Pellets with Carbon Nano-Tubes Using Spark Plasma Sintering

Uranium dioxide (UO2) is the most common fuel material in commercial nuclear power reactors. Despite its numerous advantages such as high melting point, good high-temperature stability, good chemical compatibility with cladding and coolant, and resistance to radiation, it suffers from low thermal conductivity that can result in large temperature gradients within the UO2 fuel pellet, causing it to crack and release fission gases. Thermal swelling of the pellets also limits the lifetime of UO2 fuel in the reactor. To mitigate these problems, we propose to develop novel UO2 fuel with uniformly distributed carbon nanotubes (CNTs) that can provide high-conductivity thermal pathways and can eliminate fuel cracking and fission gas release due to high temperatures. CNTs have been investigated extensively for the past decade to explore their unique physical properties and many potential applications. CNTs have high thermal conductivity (6600 W/mK for an individual single- walled CNT and >3000 W/mK for an individual multi-walled CNT) and high temperature stability up to 2800°C in vacuum and about 750°C in air. These properties make them attractive candidates in preparing nano-composites with new functional properties. The objective of the proposed research is to develop high thermal conductivity of UO2–CNT composites without affecting the neutronic property of UO2 significantly. The concept of this goal is to utilize a rapid sintering method (5–15 min) called spark plasma sintering (SPS) in which a mixture of CNTs and UO2 powder are used to make composites with different volume fractions of CNTs. Incorporation of these nanoscale materials plays a fundamentally critical role in controlling the performance and stability of UO2 fuel. We will use a novel in situ growth process to grow CNTs on UO2 particles for rapid sintering and develop UO2-CNT composites. This method is expected to provide a uniform distribution of CNTs at various volume fractions so that a high thermally conductive UO2-CNT composite is obtained with a minimal volume fraction of CNTs. The mixtures are sintered in the SPS facility at a range of temperatures, pressures, and time durations so as to identify the optimal processing conditions to obtain the desired microstructure of sintered UO2-CNT pellets. The second objective of the proposed work is to identify the optimal volume fraction of CNTs in the microstructure of the composites that provides the desired high thermal conductivity yet retaining the mechanical strength required for efficient function as a reactor fuel. We will systematically study the resulting microstructure (grain size, porosity, distribution of CNTs, etc.) obtained at various SPS processing conditions using optical microscopy, scanning electron microscopy (SEM), and transmission electron microscope (TEM). We will conduct indentation hardness measurements and uniaxial strength measurements as a function of volume fraction of CNTs to determine the mechanical strength and compare them to the properties of UO2. The fracture surfaces will be studied to determine the fracture characteristics that may relate to the observed cracking during service. Finally, we will perform thermal conductivity measurements on all the composites up to 1000° C. This study will relate the microstructure, mechanical properties, and thermal properties at various volume fractions of CNTs. The overall intent is to identify optimal processing conditions that will provide a well-consolidated compact with optimal microstructure and thermo-mechanical properties. The deliverables include: (1) fully characterized UO2-CNT composite with optimal CNT volume fraction and high thermal conductivity and (2) processing conditions for production of UO2-CNT composite pellets using SPS method.

Subhash, Ghatu↗
DOE OSTI2018

Apparent Fracture Toughness of Pressureless Sintered Silver Interconnects

This study uses three-point flexural testing to estimate the room-temperature apparent fracture toughness ( K Ic_app ) of a pressureless sintered-silver interconnect - a candidate material for use in power electronic devices. The K Ic_app estimation occurs via work-of-fracture measurement of a chevron-shaped sintered-silver joint centrally located in an “interconnect bend test specimen”. The chevron-shape was stencil-printed on a silver (Ag)-plated direct bonded copper (DBC) substrate, mated to an Ag-plated DBC substrate, and then sintered. The chevron-shape, used for decades in fracture mechanics examinations and in standardized tests of monolithic materials, enables controlled stable crack initiation and propagation that are prerequisites for valid K Ic_app estimation. The employed combination of an interconnect bend test specimen and bend test method is robust and simple, enables a means for interpreting the resistance to crack growth and delamination in an interconnect, provides a dependable way to judge the efficacies of sintered-silver processing conditions, and ultimately supports process optimization of sintered-silver interconnects.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Double-Sided Pressureless-Sintered-Silver Interconnects Fabricated by Reflow-Oven-Processing

A significant amount of development with sintered-silver as an alternative interconnect (or attachment or attach) material in power electronic devices has occurred since ~ 2010 at Oak Ridge National Laboratory's National Transportation Research Center. Continuous sponsorship of the work enabled improvements and understanding of several sequential processing steps which otherwise would not have occurred with a short duration or an intermittently funded project. The majority of that work has occurred with a focus on improving its processing and consequential mechanical reliability of the interconnect while promoting adaptability to power elect ronic device manufacturing. The work includes determining application issues of silver-sintering and the developing processes that would make it amenable for use with reflow oven sintering. As part of that work, co-development of maximum interconnect strength of the sintered-silver interconnect occurred, and that also involved examining candidate plating materials that could be used in concert with them for the "interconnect system". All of this work involved the consideration of a single sintered-silver interconnect.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Fundamentals of Spark-Plasma Sintering (Final Report)

This project was focused on the development of the general theory of spark-plasma sintering (SPS) taking into account the role of both thermal and non-thermal factors in the acceleration of SPS mass transport. SPS is a particular kind of field-assisted sintering, which provides potentially revolutionary capabilities to the processing of materials into configurations previously unattainable. This approach significantly improves the processing time- and quality-wise. It carries the potential of maintaining the nano and sub-micron structure in nano-powder-based materials after consolidation. SPS gains particular prominence in connection with its exceptional potential of rapid and ultra-rapid processing of very hard-to-deform materials, which would typically require lengthy consolidation times at significantly elevated temperatures under conditions of conventional powder pressing or sintering. The achievement of the ultimate goal of the formulation of the general theory of spark plasma sintering required the identification of the contributions of all the thermal and non-thermal factors in the enhancement of mass transport under SPS processing conditions. As our research indicated, this enhancement is mostly reduced to the creation of the conditions of controlled non-equilibrium, which is especially important in ultra-rapid field-assisted sintering techniques. Thus, the main project objective was the analysis of the SPS physical basis at multiple scales specifically exploring the role of electric current in the acceleration of mass transport and with an emphasis on the conditions of controlled non-equilibrium.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Mechanically Robust High Magnetic Performance Sm-Co Sintered Magnets (Final Report)

Samarium-cobalt based permanent magnets (SmCo 5 and Sm 2 Co 17 ) have excellent magnetic properties, good corrosion resistance, and long-term thermal stability. Sm-Co sintered magnets have been widely used in electric machines, telecommunication, biomedical devices, and magnetic sensors. They are the most preferred magnets for high-temperature applications (200 - 550 °C). However, Sm-Co sintered magnets are brittle. They cannot be used for applications subjected to high stress, vibration, or mechanical shock. Sm-Co sintered magnets are prone to chipping, and fracture in the course of block magnet manufacturing, part machining, assembly, and operation. The brittleness leads to a magnet production loss of up to 20-30% in volume and imposes limitations on part size and shape. Developing mechanically robust high-performance Sm-Co sintered magnets is of great scientific and technical significance. This project is in response to the current market need for mechanically robust high magnetic performance Sm-Co sintered magnets and their novel manufacturing processes. The project will focus on scaling-up, validation, and technology maturation study of the mechanically tough high magnetic performance Sm-Co magnets developed by Ames Laboratory at a lab-scale with the collaboration of the industry partner Electron Energy Corporation (EEC).

36 MATERIALS SCIENCE↗
NASA NTRS1979

Effect of oxygen-nitrogen ratio on sinterability of Sialons

The effect of varying the sintering temperature and the oxygen to nitrogen ratio (O/N) on the sinterability of Sialons of the formula Si2.55Al0.6OyN4-0.667y was investigated for y between 0.57 and 1.92 (O/N between 0.157 and 0.706). The Sialons reached maximum density on pressureless sintering for 4 hours at about 1760 C in nitrogen. Optimum sinterability with densities up to about 98 percent of theoretical was attained with negligible X-phase in the O/N range from about 0.2 to 0.3. On sintering at approximately 1830 C the Sialons decomposed with evolution of silicon and aluminum.

Arias, A.↗
NASA NTRS1983

Sintering of reaction bonded silicon nitride

A process to produce sintered reaction-bonded Si3N4 (SRBSN) articles has been developed. This process consists of the addition of an appropriate sintering aid to reaction-bonded Si3N4 followed by sintering between 1780 and 2000 C, using an over pressure of nitrogen. The principal advantage of this process is the low sintering shrinkages of 5 to 10 percent. The properties and microstructure of two SRBSN systems sintered with MgO and Y2O3 additives are described and were found to be comparable to corresponding hot-pressed Si3N4 systems. Examples of applications of both systems are illustrated, demonstrating near net shape fabrication capability of the process.

Mangels, J. A.↗
NASA NTRS1984

Reactive sintering of SiC

Investigation of the sintering processes involved in the sintering of SiC revealed a connection between the types and quantities of sintering additives or catalysts and densification, initial shrinkage, and weight loss of the sintered SiC material. By sintering processes, is meant the methods of mass transport, namely solid vapor transport and grain boundary diffusion.

Kim, Y. W.↗
NASA NTRS1986

Manufacture of high-density ceramic sinters

High density ceramic sinters are manufactured by coating premolded or presintered porous ceramics with a sealing material of high SiO2 porous glass or nitride glass and then sintering by hot isostatic pressing. The ceramics have excellent abrasion and corrosion resistances. Thus LC-10 (Si3N2 powder) and Y2O3-Al2O3 type sintering were mixed and molded to give a premolded porous ceramic (porosity 37%, relative bulk density 63%). The ceramic was dipped in a slurry containing high SiO2 porous glass and an alcohol solution of cellulose acetate and dried. The coated ceramic was treated in a nitrogen atmosphere and then sintered by hot isostatic pressing to give a dense ceramic sinter.

Hibata, Y.↗
NASA NTRS1985

Manufacture of sintered silicon nitrides

Sintered silicon nitrides are manufactured by sintering Si3N powder containing 2 to 15% in wt of a powder mixture composed of nitride powder of lanthanide or Y 100 parts and AIN powder less than 100 parts at 1500 to 1900 deg. temperature under a pressure of less than 200 Kg/sq. cm. The sintered Si3N has high mechanical strength in high temperature. Thus, Si3N4 93.0, Y 5.0 and AlN 2.0% in weight were wet mixed in acetone in N atom, molded and sintered at 1750 deg. and 1000 Kg/sq. cm. to give a sintered body having high hardness.

Iwai, T.↗
NASA NTRS1988

A sintering model for SiC(sub)w/Si3N4 composites

Presented is a model which suggests that it should be possible to pressureless sinter a SiC(sub w)/ Si3N4 composite to theoretical density. Prior failure to achieve complete densification by sintering is attributed to the use of compositions which result in a glass deficit. There is one basic premise for this model. The ratio of glass amount to surface area of nonglass constituents must be the same for both composite and sinterable monolithic Si3N4. This model suggests that whisker and grain sizes and whisker loading influence the glass amount necessary for successful sintering of composites. According to the model, a large glass amount will be necessary for successful sintering of these composites. However, grain boundary thicknesses in the composite will be less than those in the analogous monolithic materials. This suggests that good high temperature strength may still be attained. A recent report supports the predictions of the model.

Freedman, Marc R.↗
NASA NTRS1991

Thermochemical analysis of the silicon carbide-alumina reaction with reference to liquid-phase sintering of silicon carbide

The stabilities of different phases in the Si-Al-C-O system are calculated from thermodynamic considerations with the objective of identifying the liquid phases formed during sintering of SiC in the presence of Al2O3. It is shown that a liquid phase can form at the sintering temperatures by the reaction of SiC with Al2O3. Depending on the carbon activity, the liquid can be either of the following: Al2O3 + Al4C3, SiC + Al4C3, or molten aluminum. The stability of the aluminosilicate melts that can form by the reaction of Al2O3 with the surface silica layer on SiC powders is also evaluated. Several factors that influence liquid-phase sintering, such as the solubility of SiC in the melts and the generation of gases during sintering, are discussed. The results of the thermodynamic analysis are compared with the observed sintering behavior for SiC.

Misra, Ajay K.↗
NASA NTRS1993

Powder metallurgy: Solid and liquid phase sintering of copper

Basic powder metallurgy (P/M) principles and techniques are presented in this laboratory experiment. A copper based system is used since it is relatively easy to work with and is commercially important. In addition to standard solid state sintering, small quantities of low melting metals such as tin, zinc, lead, and aluminum can be added to demonstrate liquid phase sintering and alloy formation. The Taguchi Method of experimental design was used to study the effect of particle size, pressing force, sintering temperature, and sintering time. These parameters can be easily changed to incorporate liquid phase sintering effects and some guidelines for such substitutions are presented. The experiment is typically carried out over a period of three weeks.

Sheldon, Rex↗
NASA NTRS1998

Sintering and Creep Behavior of Plasma-Sprayed Zirconia and Hafnia Based Thermal Barrier Coatings

The sintering and creep of plasma-sprayed ceramic thermal barrier coatings under high temperature conditions are complex phenomena. Changes in thermomechanical and thermophysical properties and in the stress response of these coating systems as a result of the sintering and creep processes are detrimental to coating thermal fatigue resistance and performance. In this paper, the sintering characteristics of ZrO2-8wt%y2O3, ZrO2-25wt%CeO2-2.5wt%Y2O3, ZrO2-6w%NiO- 9wt%Y2O3, ZrO2-6wt%Sc2O3-2wt%y2O3 and HfO2-27wt%y2O3 coating materials were investigated using dilatometry. It was found that the HfO2-Y2O3 and baseline ZrO2-Y2O3 exhibited the best sintering resistance, while the NiO-doped ZrO2-Y2O3 showed the highest shrinkage strain rates during the tests. Higher shrinkage strain rates of the coating materials were also observed when the specimens were tested in Ar+5%H2 as compared to in air. This phenomenon was attributed to an enhanced metal cation interstitial diffusion mechanism under the reducing conditions. It is proposed that increased chemical stability of coating materials will improve the material sintering resistance.

Zhu, Dongming↗
NASA NTRS2007

Sintering of Lunar and Simulant Glass

Most oxygen-extraction techniques are temperature-dependent, with higher temperatures resulting in higher oxygen yield. An example is hydrogen reduction, in which the optimum process temperature is 1050 C. However, glass-rich lunar soil begins to show the effects of sintering at temperatures of 900 C or lower. Sintering welds particles together due to viscous relaxation of the glass in the sample. One approach to avoid problems related to sintering, such as difficulty in removing waste material from the reactor, is to keep the soil in motion. One of several methods being studied to accomplish this is fluidized-bed processing techniques, in which the grains are kept in motion by the action of flowing reductant gas. The spent material can be removed from the chamber while still fluidized, or the fluidizing motion can continue until the material has cooled below approx. 500 C. Until end-to-end prototypes are built that can remove the heated soil, the most practical option is to keep the bed fluidized while cooling the waste material. As ISRU technology advances, another option will become valuable, which is to intentionally sinter the material to a great enough extent that it becomes a brick. The free iron in lunar soil is magnetic, and ferromagnetic bricks can be manipulated by robotic systems using electromagnetic end effectors. Finally, if an electromagnetic field is applied to the soil while the brick is being formed, the brick itself will become a magnet. This property can be used to create self-aligning bricks or other building materials that do not require fasteners. Although sintering creates a challenge for early lunar surface systems, knowledge gained during prototype development will be valuable for the advanced lunar outpost.

Cooper, Bonnie L.↗
NASA NTRS2019

Optimization of Aluminum-Tin Ink Composition and Sintering in Atmospheric Conditions

This study will focus on the basics of generating an aluminum-tin ink that can sinter in air and exhibits properties near that of a solid aluminum-tin alloy. Sintering temperatures will also be assessed in this study. Once the optimal aluminum ink composition is determined, the optimal ink thickness for homogeneous sintering must be determined by additional experimentation. Additive manufacturing is a rapidly developing and growing manufacturing process and has proven successful in many different ways. Processes, such as extrusion three-dimensional (3D) printing and selective laser melting (SLM), have proven to work but have limitations, such as material capabilities or density issues. SLM is a revolutionary process for additive manufacturing of metals but cannot be used in outer space due to the need for metallic powder which would diffuse into the atmosphere in a zero-gravity environment. For this reason, metallic ink additive manufacturing is a potential solution. Work is being done on metallic ink additive manufacturing in a vacuum for electrical applications. This project has focused on developing an aluminum-tin metallic ink that can sinter without the need of a vacuum or inert gas-purged atmosphere in order to prevent oxidation of the aluminum by adding flux. Once a potential ink composition has been determined through sintering of small disks and thin layers of ink, the ink may be studied with a multimaterial 3D printer at NASA Marshall Space Flight Center (MSFC) in future experiments. If successful, this aluminum-tin ink will be capable for use on the International Space Station to make replacement parts quickly. Along with its zero-gravity advantages, this ink may also have applications on Earth because it may be extruded on a substrate with precise ceramic tips in a 3D printing process. This would allow the fabrication of precise, complex shapes and may generate a much faster and more efficient printing process as compared with traditional powder bed additive manufacturing processes. The process would not be limited by a small building volume because the system would not require an enclosed chamber.

Courtright, Z. S.↗
NASA NTRSDate not supplied

Fabrication and Characterization of A Lunar Simulant-Based Sintered Construction Material

In-situ resource utilization (ISRU) is critical to enable future efforts to have a long-term human presence on the Moon as well as Mars. ISRU technologies are being developed for radiation protection, dust mitigation, thermal insulation, and other applications. One such ISRU technology for creating construction materials out of lunar and Martian regolith is sintering, which is a thermal-based construction process that bonds finely grained material together at temperatures below the melting point. However, the conditions employed during the sintering, such as temperature, atmospheric composition, duration of the process, and pressure, can have a significant impact on the quality and strength of the resulting materials. In parallel, the development of methods for characterizing the quality, porosity, density, and other properties of these materials is critical. X-ray computed tomography (X-ray CT) can image large changes in density within a material, such as the presence of pores throughout an otherwise uniform medium, with relatively high spatial resolution. Similarly, Terahertz time-domain spectroscopic (THz-TDS) imaging is sensitive to density variations within samples, but is restricted to non-conducting materials. Specifically, previous work has shown that the refractive index (n eff ) values obtained through the analysis of THz-TDS images increases with increasing density within plastic samples. Even further, this work showed that it is possible to create a calibration curve for a given material from samples of different, but known density, which can enable one to directly convert n eff to density for samples having the same composition, but unknown density. Here, we report on the fabrication of a lunar simulant-based sintered construction material using vacuum hot pressed (VHP) sintering, then show X-ray CT and THz-TDS imaging results of the sample, which show spatial variations in the material. This has important implications for efforts to improve these types of lunar construction material processes and verify the quality of these materials in terms of consolidation. To the best of our knowledge, there is no previous work utilizing VHP sintering to make lunar simulant-based construction materials or exploring the feasibility of THz imaging to spatially map the density variation through a lunar simulant-based construction material.

Terahertz time-domain spectroscopic imaging↗