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Material for solid state sintered material

A solid state sintered material is described that includes a mixed oxide of lanthanum, strontium, cobalt, iron and oxygen, and CaCO3 inclusions. The solid state sintered material can also include calcium oxide, which can form from thermal composition of calcium carbonate. The solid state sintered material can also include a pore-forming particulate material such as carbon black and/or a doped ceramic metal oxide ionic conductor such as Sm-doped ceria uniformly dispersed in the solid state sintered material. The solid state sintered material can be formed from a two-step process in which a portion of the CaCO3 is mixed with the mixed oxide materials and heated to form porous agglomerates, and the remaining CaCO3 is added during the formation of a sintering paste. The solid state sintered material described herein can be used as a cathode material for solid oxide fuel cell.

36 MATERIALS SCIENCE↗

Computational Fluid Dynamics Simulation of a Pilot-Scale Waste Glass Melter

The INL has been developing a high-fidelity computational fluid dynamics (CFD) model of a Joule-heated ceramic-lined waste glass melter. The purpose is to better understand the dynamics of heat transfer within the system, in order to provide support for the optimization of the Hanford Waste Treatment Plant (WTP) that will be used for vitrification of legacy tank waste. The simulation presented here is for the DM1200 pilot-scale system, which has been operated by the Vitreous State Laboratory (VSL) over the past several decades. This system is about one-third of the scale of the full size WTP melter. Experimental data from this system is being used to validate computational simulations. The examination of the melter with a fully coupled CFD model should give an accurate assessment of the heat transfer into the reactive cold cap region. Heat is provided to the cold cap region from conduction and convection from the molten glass pool as well as radiation from the hot plenum above the cold cap. The CFD model implements a mathematical model of the cold cap developed for the assessment of the melting rate during the vitrification of tank waste. This sub-model implemented directly into the CFD model combines the mass and enthalpy balance of the cold cap together with the conversion kinetics of the feed. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Potential for EMU Fabric Damage by Electron Beam and Molten Metal During Space Welding for the International Space Welding Experiment

As a consequence of preparations concerning the International Space Welding Experiment (ISWE), studies were performed to better understand the effect of molten metal contact and electron beam impingement with various fabrics for space suit applications. The question arose as to what would occur if the electron beam from the Ukrainian Universal Hand Tool (UHT) designed for welding in space were to impinge upon a piece of Nextel AF-62 ceramic cloth designed to withstand temperatures up to 1427 C. The expectation was that the electron beam would lay down a static charge pattern with no damage to the ceramic fabric. The electron beam is capable of spraying the fabric with enough negative charge to repel further electrons from the fabric before significant heating occurs. The static charge pattern would deflect any further charge accumulation except for a small initial amount of leakage to the grounded surface of the welder. However, when studies were made of the effect of the electron beam on the insulating ceramic fabric it was surprisingly found that the electron beam did indeed burn through the ceramic fabric. It was also found that the shorter electron beam standoff distances had longer burnthrough times than did some greater electron beam standoff distances. A possible explanation for the longer burnthrough times for the small electron beam standoff distance would be outgassing of the fabric which caused the electron beam hand-tool to cycle on and off to provide some protection for the cathodes. The electron beam hand tool was observed to cycle off at the short standoff distance of two inches likely due to vapors being outgassed. During the electron beam welding process there is an electron leakage, or current leakage, flow from the fabric. A static charge pattern is initially laid down by the electron beam current flow. The static charge makes up the current leakage flow which initially slightly heats up the fabric. The initially laid down surface charge leaks a small amount of current. The rate at which the current charge leaks from the fabric controls how fast the fabric heats up. As the ceramic fabric is heated it begins to outgass primarily from contamination/impurities atoms or molecules on and below the fabric surface. The contaminant gases ionize to create extra charge carriers and multiply a current of electrons. The emitted gas which ionized in the electron leakage flow promotes further leakage. Thus, the small leakage of charge from the fabric surface is enhanced by outgassing. When the electron beam current makes up the lost current, the incoming electrons heat the fabric and further enhance the outgassing. The additional leakage promotes additional heating up of the ceramic fabric. The electrons bound to the ceramic fabric surface leak off more and more as the surface gets hotter promoting even greater leakage. The additional electrons that result also gain energy in the field and produce further electrons. Eventually the process becomes unstable and accelerates to the point where a hole is burned through the fabric.

Fragomeni, James M.↗

Investigating ceramic breeder pebble beds thermomechanics evolution using novel pressure mapping technology

Ceramic breeder pebble beds undergo complex thermomechanical interactions during blanket operation due to stress build-up and relaxation under the effects of confined thermal expansion, thermal cycling, and creep. Understanding the evolution of such processes can aid in guiding blanket design/assembly, breeder materials developments, predicting performance and possible failure modes. This study introduces experimental techniques that enable us to create an environment in which the pebble bed stresses are organically generated as a result of relevant temperature gradients and magnitudes that allows us to observe the combined thermomechanical interaction effects. A novel non-intrusive in-situ tactile pressure sensing technology is used to generate real-time contact pressure maps revealing the spatial and temporal stress evolution with emphasis on understanding the roles that each of the thermo-mechanical forces play in dictating the pebble bed’s equilibrium conditions. Two types of bed-wall contact pressure drop were recorded: (1) within the subsequent cycles due to pebbles irreversible rearrangements, and (2) within the cycle itself as a result of creep/stress-relaxation. Consequently, by the fourth cycle, the contact pressure drops to negligible values and remains stable. This stability is attributed to two modes of self-regulation: (1) stress self-regulation as a result of pressure rise and fall due to thermal expansion and creep/thermal cycling, respectively, and (2) temperature self-regulation due to the locally enhanced thermal conductivity in the core region of the bed accompanied by deteriorated interface conductance. These two mechanisms are desirable as they lower the probability of the events of pebbles crushing and thermal runaways under high temperatures/stresses and poor heat extraction.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

Green micromachining of ceramics using tungsten carbide micro-endmills

This paper presents an experimental analysis on micromachining of green-state silicon carbide (SiC) and aluminum nitride (AlN) using uncoated tungsten carbide (WC) micro-endmills. Although the unique properties of ceramics make them ideal materials for many applications involving micro-scale features, the industrial adaptation of ceramics at the micro-scale has been hindered due to the lack of viable ceramic micro-manufacturing techniques. Green micromachining (GMM), where micro-scale features are created by micromachining green-state ceramics that contain ceramic particles and a polymer binder, offers a potential solution for this problem by affording tremendous improvements in micromachinability with respect to sintered ceramics. After the completion of GMM, the green parts are debound and sintered to obtain the final component with the desired microscale features. In this work, we evaluated GMM characteristics of powder-injection molded green-state SiC and AlN to correlate process conditions and green-material compositions with the micromachining forces, quality, and tool wear. An experimental study that involves full immersion micromilling tests with 254 μm diameter micro-endmills at different cutting speeds and feed rates is conducted. For each of the two materials, two binder states (with and without wax) and two powder states (with micro particles only, or with both micro- and nanoparticles) are investigated. Green micromachining forces, specific energies and the resulting surface roughness are analyzed quantitatively. A qualitative analysis of burr formation and channel quality, as well as a preliminary study on micro-tool wear are also performed. Both the machining conditions and the material compositions are seen to have a strong effect on micro-machinability of green-state ceramics. Overall, we conclude that GMM can be a viable ceramic micro-manufacturing strategy if favorable (or optimal) micromachining and material parameters are identified through the presented (or a similar) micromachinability study.

36 MATERIALS SCIENCE↗

Production of LEU fully ceramic microencapsulated fuel for irradiation testing

The Advanced Fuels Campaign of the US DOE Fuel Cycle Research/Development program is currently engaged in production of FCM fuel for irradiation testing in the Advanced Test Reactor (ATR) at Idaho National Laboratory (INL). FCM fuel production is a serial process with 3 major steps namely kernel, TRISO, and compact production. The first step in the kernel process is production of air-dried UO{sub 3} gel spheres with suspended carbon particles. These spheres, roughly 2 mm in size, are then calcined to produce a mixture of UO{sub 2} and carbon. This calcination step may be performed in either argon, hydrogen, or mixtures of these gases. Once the calcination step is complete, temperature is increased (>1400 Celsius degrees) to convert this mixture to UO{sub 2} + UC{sub x}. Once dense oxide-carbide kernels are available, the inert environment is switched to a nitrogen containing one to facilitate carbothermic reduction of kernels and production of UN. Essentially, the oxygen and carbon in the oxide-carbide kernels react with one another to produce CO and are replaced with nitrogen inside the lattice. The TRISO step in fuel production is incorporation of a porous carbon buffer layer, a dense inner pyrolytic carbon layer (IPyC), a SiC layer, and finally and outer pyrolytic carbon layer (OPyC) onto the UN kernels. The coating layer deposition step is carried out inside a graphite furnace using a fluidized bed chemical vapor deposition (CVD) process. In essence, a mixture of reactant and inert gasses flow from the bottom through a bed of particles that are in turn fluidized by the gas stream. The particles undergo CVD and once a different coating layer is to be incorporated, the furnace temperature is adjusted and the reactant gases are changed. The final step in the series of fuel production activities is the consolidation of UN TRISO particles inside the SiC matrix to produce cylindrical pellets. It entails 3 critical areas: SiC powder mixing, over-coating of particles, and high-temperature densification. Optimal execution of the powder mixing step is vital to achieve a fully dense SiC matrix at the end of the process. The SiC matrix is consolidated using a special form of liquid phase sintering (LPS) involving nano-powder feedstock that is designated as the NITE process. The SiC nano-powder slurry is sprayed directly onto the particle surface using a piezoelectric nozzle. Once the over-coated particles are available, final consolidation step at high temperatures (1875 Celsius degrees) is carried out.

36 MATERIALS SCIENCE↗

Intermetallic and ceramic matrix composites for 815 to 1370 C (1500 to 2500 F) gas turbine engine applications

Light weight and potential high temperature capability of intermetallic compounds, such as the aluminides, and structural ceramics, such as the carbides and nitrides, make these materials attractive for gas turbine engine applications. In terms of specific fuel consumption and specific thrust, revolutionary improvements over current technology are being sought by realizing the potential of these materials through their use as matrices combined with high strength, high temperature fibers. The U.S. along with other countries throughout the world have major research and development programs underway to characterize these composites materials; improve their reliability; identify and develop new processing techniques, new matrix compositions, and new fiber compositions; and to predict their life and failure mechanisms under engine operating conditions. The status is summarized of NASA's Advanced High Temperature Engine Materials Technology Program (HITEMP) and the potential benefits are described to be gained in 21st century transport aircraft by utilizing intermetallic and ceramic matrix composite materials.

Stephens, Joseph R.↗

An Advanced Extreme-Environment Wireless Telemetry System for Turbine Blade Instrumentation

As advanced natural gas power generation systems evolve, the thrust for increased efficiencies and reduced emissions results in increasingly harsh conditions inside the turbine environment. These high temperatures, pressures, and corrosive atmospheres result in accelerated rates of degradation, leading to failure of turbine materials and components. Wolfspeed, A Cree Company, Siemens Energy, and Siemens Corporate Technology, in collaboration with the Department of Energy (DOE)'s National Energy Technology Laboratory, are developing a reliable and long-term monitoring capability in the turbine hot gas path in the form of novel ceramic-based thermocouples and wide bandgap instrumentation electronics that will contribute to the overall reliability of gas turbines. When equipped with better monitoring and controls, power plants can operate with increased fuel-burning efficiency, improved process dynamics and gas concentrations, and increased overall longevity of the power plant components. This will result in increased turbine availability and a reduction in outages and maintenance costs. The technology being developed in this program is based on advanced techniques and innovations in nearly every aspect of high-temperature electronics, including materials, semiconductor devices, subcomponents, electronic packaging, and system integration. The environment in which this wireless system must operate has continuous centrifugal loads with a gravitation force on the order of 16,000 times the force of gravity (16,000 g) and temperatures exceeding 400°C. This article will specifically discuss the background and motivation for the high-temperature instrumentation system and will explain the high-level electrical system, the construction of the instrumentation package, the techniques used for integration onto rotating components, as well as the wireless power and data transmission systems. In addition to the electrical and mechanical design, this article will also discuss results from laboratory bench testing as well as heated spin rig testing. Lastly, this article will highlight the future direction of the instrumentation system evolution, with a final objective of insertion into Siemens natural gas turbine power plants.

47 OTHER INSTRUMENTATION↗

Hail Monitor Sensor

An inexpensive and simple hail monitor design has been developed that has a single piezoelectric ceramic disc and uses a metal plate as a sounding board. The structure is durable and able to withstand the launch environment. This design has several advantages over a multi-ceramic sensor, including reduced cost and complexity, increased durability, and improvement in impact response uniformity over the active surface. However, the most important characteristic of this design is the potential to use frequency discrimination between the spectrum created from raindrop impact and a hailstone impact. The sound of hail hitting a metal plate is distinctly different from the sound of rain hitting the same plate. This fortuitous behavior of the pyramid sensor may lead to a signal processing strategy, which is inherently more reliable than one depending on amplitude processing only. The initial concept has been im proved by forming a shallow pyramid structure so that hail is encouraged to bounce away from the sensor so as not to be counted more than once. The sloped surface also discourages water from collecting. Additionally, the final prototype version includes a mounting box for the piezo-ceramic, which is offset from the pyramid apex, thus helping to reduce non-uniform response (see Figure 2). The frequency spectra from a single raindrop impact and a single ice ball impact have been compared. The most notable feature of the frequency resonant peaks is the ratio of the 5.2 kHz to 3.1 kHz components. In the case of a raindrop, this ratio is very small. But in the case of an ice ball, the ratio is roughly one third. This frequency signature of ice balls should provide a robust method for discriminating raindrops from hailstones. Considering that hail size distributions (HSDs) and fall rates are roughly 1 percent that of rainfall, hailstone sizes range from a few tenths of a centimeter to several centimeters. There may be considerable size overlap between large rain and small hail. As hail occurs infrequently at KSC, the ideal HSD measurement sensor needs to have a collection area roughly 100 times greater than a raindrop-size distribution sensor or disdrometer. The sensitivity should be such that it can detect and count very small hail in the midst of intense rainfall consisting of large raindrop sizes. The dynamic range and durability should allow measurement of the largest hail sizes, and the operation and calibration strategy should consider the infrequent occurrence of hail fall over the KSC area.

Younquist, Robert↗

Fabrication and Testing of a Novel Ceramic-Based Additively Manufactured Humidity Sensor

A material capable of detecting minute changes in ambient humidity via a change in its electrical properties is critical to enabling the success of vapor-sensitive components on Earth and abroad. Manufacturing of these hydrophilic materials currently follows an extensive process of heat treating focused on removing the solvent and organic vehicle. This research aims to reduce the complexity of manufacturing these novel sensors by eliminating the high-temperature (>850 °C) processing stages. A method based on printing a polymer embedded with hydrophilic nanoparticles is accomplished through selected additively manufactured methods. This research branches into the elimination of physical spare parts with the ability to print highly sensitive in-situ sensors, reducing the environmental footprint in space-critical environments like the International Space Station (ISS).

sensor↗

A Model of Grain Boundary Complexion Transitions and Grain Growth in Yttria-Doped Alumina

In this work, we present a physically-parameterized microstructure evolution model for the Yttria-doped alumina system. Yttria-doped alumina is a well-known ceramic system which undergoes first-order phase-like transitions at grain boundaries, which can radically alter interface properties. The change in interfacial properties in turn can radically change microstructure outcomes during processing, including the induction of abnormal grain growth modes. In this work, we develop a simulation that evolves alumina microstructure as a function of yttria concentration and temperature. In the window studied, we achieve strong agreement with reviewed experimental results in identifying the windows for large grains, small grains, abnormal grain growth, and complexion transition kinetics. We then apply the model to study and demonstrate how the possible inclusion of second-phase particles or uneven solute distribution profiles will impact microstructure evolution. It is found that particles do not significantly affect abnormal grain growth in the window studied (but do lead to reduced grain size through pinning effects). It is found that even modest amounts of solute inhomogeneity will result in substantial changes in microstructure outcomes, frequently leading to clusters of abnormal grains. This model largely corroborates the expectations and hypotheses made from recent experimental studies in oxide-doped alumina systems. Further, it is found that there exists a peak transition fraction for the system at which abnormal grain size tends to be maximized.

Grain Growth, Grain Boundary Complexion, abnormal ↗

Additive manufacturing of hybrid circuits

There is a rising interest in developing functional electronics using additively manufactured components. Considerations in materials selection and pathways to forming hybrid circuits and devices must demonstrate useful electronic function; must enable integration; and must complement the complex shape, low cost, high volume, and high functionality of structural but generally electronically passive additively manufactured components. This article reviews several emerging technologies being used in industry and research/development to provide integration advantages of fabricating multilayer hybrid circuits or devices. First, we review a maskless, noncontact, direct write (DW) technology that excels in the deposition of metallic colloid inks for electrical interconnects. Second, we review a complementary technology, aerosol deposition (AD), which excels in the deposition of metallic and ceramic powder as consolidated, thick conformal coatings and is additionally patternable through masking. As a result, we show examples of hybrid circuits/devices integrated beyond 2-D planes, using combinations of DW or AD processes and conventional, established processes.

36 MATERIALS SCIENCE↗

Quantitative Ultrasonic Evaluation of Mechanical Properties of Engineering Materials

Progress in the application of ultrasonic techniques to nondestructive measurement of mechanical strength of engineering materials is reviewed. A dormant concept in nondestructive evaluation (NDE) is invoked. The availability of ultrasonic methods that can be applied to actual parts to assess their potential susceptibility to failure under design conditions is discussed. It was shown that ultrasonic methods yield measurements of elastic moduli, microstructure, hardness, fracture toughness, tensile strength, yield strength, and shear strength for a wide range of materials (including many types of metals, ceramics, and fiber composites). It was also indicated that although most of these methods were shown feasible in laboratory studies, more work is needed before they can be used on actual parts in processing, assembly, inspection, and maintenance lines.

Vary, A.↗

Microgravity science and applications bibliography, 1984 revision

A compilation of Government reports, contractor reports, conference proceedings, and journal articles dealing is presented that deal with flight experiments utilizing a low gravity environment to elucidate and control various processes or with ground based activities that provide supporting research. Subdivisions include six major categories: (1) Electronic Materials; (2) Metals, Alloys, and Composites; (3) Fluid Dynamics and Transports; (4) Biotechnology; (5) Glasses and Ceramics; and (6) Combustion. Also included are publications from the European, Soviet, and Japanese MSA programs. In addition, there is a list of patents and appendices providing a compilation of anonymously authored reports and a cross reference index.

Pentecost, E.↗

Factors Affecting Fiber Design and Selection for Advanced Ceramic Composites

Structural Ceramic Matrix Composites (CMC) have the potential for application in the hot sections of a variety of advanced propulsion and power systems. It is therefore necessary to have a general understanding of the key properties of CMC and Reinforcing Fibers. This need is complicated by the wide variety of application conditions and structural requirements for which CMC's will be used, and the proprietary concerns of the design engineers. CMC's, to be successful, must display properties which are competitive with the currently used high temperature structural materials: (i.e., Iron and Nickel based superalloys, tough monolithic ceramics, and carbon/carbon composites.) Structural CMC offers several areas of competition: (1) performance, (i.e., strength and strength retention, creep resistance, and thermal conductivity), (2) reliability (i.e., environmental durability, and damage tolerance) and (3) processing (i.e., capability for varying sizes and shapes, and cost effective fabrication). The presentation further discusses, and illustrates with fiber and CMC data the key fiber properties and processes which strongly affect each CMC area of competition. The presentation further discusses the current knowledge of the important factors which control the key fiber properties. A design guidelines for the optimum fiber characteristics is developed, and the currently available fibers are compared against those guidelines.

DiCarlo, James A.↗

Polymer/Silicate Nanocomposites Developed for Improved Thermal Stability and Barrier Properties

The nanoscale reinforcement of polymers is becoming an attractive means of improving the properties and stability of polymers. Polymer-silicate nanocomposites are a relatively new class of materials with phase dimensions typically on the order of a few nanometers. Because of their nanometer-size features, nanocomposites possess unique properties typically not shared by more conventional composites. Polymer-layered silicate nanocomposites can attain a certain degree of stiffness, strength, and barrier properties with far less ceramic content than comparable glass- or mineral-reinforced polymers. Reinforcement of existing and new polyimides by this method offers an opportunity to greatly improve existing polymer properties without altering current synthetic or processing procedures.

Campbell, Sandi G.↗

Electrical Resistance Technique to Monitor SiC Composite Detection

Ceramic matrix composites are suitable for high temperature structural applications such as turbine airfoils and hypersonic thermal protection systems. The employment of these materials in such applications is limited by the ability to process components reliable and to accurately monitor and predict damage evolution that leads to failure under stressed-oxidation conditions. Current nondestructive methods such as ultrasound, x-ray, and thermal imaging are limited in their ability to quantify small scale, transverse, in-plane, matrix cracks developed over long-time creep and fatigue conditions. Electrical resistance of SiC/SiC composites is one technique that shows special promise towards this end. Since both the matrix and the fibers are conductive, changes in matrix or fiber properties should relate to changes in electrical conductivity along the length of a specimen or part. The effect of matrix cracking on electrical resistivity for several composite systems will be presented and some initial measurements performed at elevated temperatures under stress-rupture conditions. The implications towards electrical resistance as a technique applied to composite processing, damage detection (health monitoring), and life-modeling will be discussed.

Smith, Craig↗

An Advanced Extreme Environment Wireless Telemetry System for Turbine Blade Instrumentation

As advanced natural gas power generation systems evolve, the thrust for increased efficiencies and reduced emissions results in increasingly harsh conditions inside the turbine environment. These high temperatures, pressures, and corrosive atmospheres result in accelerated rates of degradation, leading to failure of turbine materials and components. The University of Arkansas (UA) and Siemens, in collaboration with the DoE's National Energy Technology Laboratory (NETL), are developing a reliable and long-term monitoring capability in the turbine hot gas path in the form of novel ceramic-based thermocouples and integrated wide band gap instrumentation electronics that will contribute to the overall reliability of gas turbines. When equipped with better monitoring and controls, power plants can operate with increased fuel-burning efficiency, improved process dynamics and gas concentrations, and increased overall longevity of the power plant components. This will result in increased turbine availability and a reduction in outages and maintenance costs. One of the key aspects to driving forward turbine monitoring capability is the development of high temperature capable integrated circuit (IC) electronics. Previous papers have described 500 °C + electronics that were developed primarily from a combination of discrete single transistors combined with supporting high temperature passive components. While these circuits have been tested successfully in high temperature spin test environments, the move to an IC approach will greatly increase the performance and reliability of turbine monitoring systems. This program is developing such capability through the implementation of silicon carbide (SiC) based ICs, and this paper details the initial approach and early testing of the developed devices. This research represents an important step towards the realization of a field deployable high reliability turbine condition monitoring system.

47 OTHER INSTRUMENTATION↗