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At least 973 records · Page 54

Solid Free-Form Fabrication of Continuous Fiber Reinforced Composites for Propulsion Application

For propulsion related applications, materials must be able to demonstrate excellent ablation and oxidation resistance at temperature approaching 3500 C, adequate load bearing capabilities, non-catastrophic failure modes, and ability to withstand transient thermal shock. A potential list of propulsion-material property requirements includes, low density, high elastic modulus, low thermal-expansion coefficient, high thermal conductivity, excellent erosion and oxidation/corrosion resistance, and flaw-insensitivity. In many cases, they will also need to be able to be joined, survive thermal cycling and multi-axial stress states, and for reusable applications, the materials must maintain the above attributes after prolonged exposure to extremely harsh chemical environments. The final and possibly most important attribute for these materials are the need to be lower cost and readily available in large quantities. Recently, Advanced Ceramics Research, Inc. (ACR) has developed low cost, flexible-manufacturing processes for Zr & Hf-based carbon fiber reinforced composites, materials with good oxidation and ablation resistance up to 3500 C. This process, called Continuous Composite Co-extrusion (C(sup 3)), incorporates carbon fibers to fabricate 'in-situ' carbide and boride-matrix/carbon fiber composites. M is a variation of ACR's manufacturing process for low-cost structural ceramic materials called Fibrous Monoliths with carbon fiber reinforcements. Fibrous Monolithic materials have a distinct fibrous texture, consist of intertwined cells of a primary phase, separated by cell boundaries of a tailored secondary phase and show very high fracture energies, damage tolerance, and graceful failure. Since they are monolithic powder based composites; they can be manufactured by conventional powder processing techniques using inexpensive raw materials. This combination of high performance and low cost is a breakthrough that could enable wider application of ceramics in high temperature applications. Typical volume fractions of the two phases are 80 to 95% for the cell phase and 5 to 20% for the interpenetrating cell boundary phase. ACR is currently developing an innovative solid freeform form fabrication (SFF) approach to produce Hf and Zr based ceramic composite components reinforced with continuous carbon fiber tows for critical structural components such as tubes and blisks. The process is simple, robust and will be widely applicable to a number of material systems. This technique was originally developed at the University of Delaware Center for Composite Materials (UD-CCM) for rapid fabrication of polymer matrix composites by a technique called automated tow placement or ATP. The current process is being developed in collaboration with UD-CCM. The paper will detail the freeform fabrication process to create low-cost ceramic fiber reinforced composites for high-temperature applications. The results of mechanical properties and microstructural characterization will be presented, together with examples of complex shapes and parts. It is believed that the process will be able to create complex shaped parts for propulsion applications at an order of magnitude lower cost than current CVI and PIP processes.

Vaidyanathan, R.↗

The Influence of Interfacial Roughness on Fiber Sliding in Oxide Composites with La-Monazite Interphases

Room temperature debonding and sliding of La-Monazite coated fibers is assessed using a composite with a polycrystalline alumina matrix and fibers of several different single crystal (mullite, sapphire) and directionally solidified eutectic (Al2O3/Y3Al5O12 and Al2O3/Y-ZrO2) compositions. These fibers provide a range of residual stresses and interfacial roughnesses. Sliding occurred over a debond crack at the fiber-coating interface when the sliding displacement and surface roughness were relatively small. At large sliding displacements with relatively rough interfaces, the monazite coatings were deformed extensively by fracture, dislocations and occasional twinning, whereas the fibers were undamaged. Dense, fine-grained (10 nm) microstructures suggestive of dynamic recrystallization were also observed in the coatings. Frictional heating during sliding is assessed. The possibility of low temperature recrystallization is discussed in the light of the known resistance of monazite to radiation damage. The ability of La-Monazite to undergo plastic deformation relatively easily at low temperatures may be enabling for its use as a composite interface.

Davis, J. B.↗

Fundamental Studies of Tritium Diffusivity in Pure and Defective Zircaloy-4 Getters (Tritium Science Program FY2020 Report)

Zirconium (Zr) alloys are extensively used as tritium (T) getters in nuclear reactors due to their low absorption cross section to thermal neutron, good mechanical properties at high temperature and resistant to corrosion in different environmental conditions. Zr alloys have better thermal properties than many other refractory alloys including stainless steel. The nuclear characteristic is simulated, and T is produced in tritium-producing burnable absorber rods (TPBAR) by the irradiation of neutron flux in pressurized water reactor (PWR). T thus produced diffuses through the pellets and is captured by the getter where it chemically reacts with Zr to form metal hydride (ZrTx). These hydrides are brittle and affect adversely the mechanical properties of alloys. In addition to that, mismatch in the lattice structures after hydride formation creates a stress which needs to be considered in component design and their life evaluation. Therefore, understanding the behavior of T and its species becomes significant as fuel burnup is increased, which leads to increase in hydrogen pickup and oxide formation. The transport of T and its species in pure Zr alloys, and in alloys with certain alloying elements and defects are important to understand in order to enhance the performance of the materials.

36 MATERIALS SCIENCE↗

Thermal shock testing for assuring reliability of glass-sealed microelectronic packages

Tests were performed to determine if thermal shocking is destructive to glass-to-metal seal microelectronic packages and if thermal shock step stressing can compare package reliabilities. Thermal shocking was shown to be not destructive to highly reliable glass seals. Pin-pull tests used to compare the interfacial pin glass strengths showed no differences between thermal shocked and not-thermal shocked headers. A 'critical stress resistance temperature' was not exhibited by the 14 pin Dual In-line Package (DIP) headers evaluated. Headers manufactured in cryogenic nitrogen based and exothermically generated atmospheres showed differences in as-received leak rates, residual oxide depths and pin glass interfacial strengths; these were caused by the different manufacturing methods, in particular, by the chemically etched pins used by one manufacturer. Both header types passed thermal shock tests to temperature differentials of 646 C. The sensitivity of helium leak rate measurements was improved up to 70 percent by baking headers for two hours at 200 C after thermal shocking.

Thomas, Walter B., III↗

Influence of Thermally-Grown Oxide (TGO) Layer on the Driving Forces Associated with Failure in Environmental Barrier Coating (EBC) Systems

Environmental barrier coatings (EBC) is an enabling technology for the successful application of ceramic matrix composites (CMCs) in air-breathing gas turbine engines. Spallation of environmental barrier coating (EBC) induced by thermally grown oxide (TGO) layer is a key EBC failure mode. The TGO layer, resulting from steam oxidation, grows either from a silicon bond coat layer (if present) or from the silicon carbide (SiC) based substrate itself. Critical thickness of the TGO layer for failure is in the range of 20-30 microns but it can vary due to exposure temperature, microstructure etc. Current work at NASA Glenn Research Center, under the Revolutionary Tools and Methods (RTM) project is aimed at addressing associated failure modes in EBC systems and developing robust analysis tools to aid in the design/analysis of these systems. The objective of the current work is to conduct a sensitivity study to examine the influence of uniformly and non-uniformly grown oxide layers with or without damage on the associated driving forces leading to spallation of the EBC when subjected to isothermal loading. Initial results indicate that the presence of damage (vertical cracks caused by in-plane stresses) enhances the stresses that are present due to non-uniformity. However, the presence of non-uniformity itself is still the main factor influencing the magnitude of peel and shear stresses in the TGO layer.

Mital, Subodh K.↗

Effects of CMAS Application on the Isothermal and Gradient Thermal Cycling Behavior of a Yb 2 Si 2 O 7 EBC

Environmental barrier coatings (EBCs) are critical to the continued advancement of gas turbine hot section materials technology. EBCs are required to protect Si-based ceramics such as silicon carbide fiber-reinforced silicon carbide (SiC/SiC) ceramic matrix composites (CMCs) from oxidation and corrosion in the combustion environment. One of the current challenges concerning EBC lifetime is the thermochemical reactions between calcium-magnesium-aluminosilicate (CMAS) deposits and the EBC that leads to changes in both composition and stress state. These changes can severely reduce the integrity of the EBC leading to crack formation, delamination, and spallation. Current techniques for evaluating CMAS in the laboratory rely on the pre-application of CMAS. Two commonly used application methods to deposit CMAS on EBC materials are tape-casting and air spray. In both methods, the CMAS is applied to the EBC surface at ambient temperature, and then subject to a heat treatment process for binder burnout. The purpose of this study is to compare the tape-cast and air spray methods on the CMAS corrosion of an ytterbium disilicate (Yb 2 Si 2 O 7 ) EBC subject to isothermal, and gradient thermal cycling. The results highlight if any differences exist in the CMAS infiltration kinetics between the two application methods.

Environmental barrier coatings (EBCs)↗

Thixotropy, antithixotropy, and viscoelasticity in hysteresis

Thixotropy, antithixotropy, and viscoelasticity are three types of time-dependent dynamics that involve fundamentally different underlying physical processes. Here, we show that the three dynamics exhibit different signatures in hysteresis by examining the fingerprints of the simplest thixotropic kinetic model, a new antithixotropic model that we introduce here, and the Giesekus model. We start by showing that a consistent protocol to generate hysteresis loops is a discrete shear-rate controlled ramp that begins and ends at high shear rates, rather than at low shear rates. Using this protocol, we identify two distinguishing features in the resulting stress versus shear rate loops. The first is the direction of the hysteresis loops: clockwise for thixotropy, but counterclockwise for viscoelasticity and antithixotropy. A second feature is achieved at high ramping rates where all responses lose hysteresis: the viscoelastic response shows a stress plateau at low shear rates due to lack of stress relaxation, whereas the thixotropic and antithixotropic responses are purely viscous with minimal shear thinning or thickening. We establish further evidence for these signatures by experimentally measuring the hysteresis of Laponite suspensions, carbon black suspensions, and poly(ethylene oxide) solutions, each representing a historically accepted example of each class of material behavior. The signatures measured in experiments are consistent with those predicted by the three models. This study reveals different fingerprints in hysteresis loops associated with thixotropy, antithixotropy, and viscoelasticity, which may be helpful in distinguishing the three time-dependent responses.

Mechanics↗

Predicted inlet gas temperatures for tungsten fiber reinforced superalloy turbine blades

Tungsten fiber reinforced superalloy composite (TFRS) impingement cooled turbine blade inlet gas temperatures were calculated taking into account material spanwise strength, thermal conductivity, material oxidation resistance, fiber-matrix interaction, and coolant flow. Measured values of TFRS thermal conductivities are presented. Calculations indicate that blades made of 30 volume percent fiber content TFRS having a 12,000 N-m/kg stress-to-density ratio while operating at 40 atmospheres and a 0.06 coolant flow ratio could permit a turbine blade inlet gas temperature of over 1900K. This is more than 150K greater than similar superalloy blades.

Winsa, E. A.↗

Predicted inlet gas temperatures for tungsten fiber reinforced superalloy turbine blades

Tungsten fiber-reinforced superalloy composite (TFRS) impingement-cooled turbine blade inlet gas temperatures were calculated taking into account material spanwise strength, thermal conductivity, material oxidation resistance, fiber-matrix interaction, and coolant flow. Measured values of TFRS thermal conductivities are presented. Calculations indicate that blades made of 30 volume percent fiber content TFRS having a 12,000 N-m/kg stress-to-density ratio while operating at 40 atm and a 0.06 coolant flow ratio could permit a turbine blade inlet gas temperature of over 1900 K. This is more than 150 K greater than similar superalloy blades.

Winsa, E. A.↗

Finite element analysis of thermal barrier coatings

The near-term objective is to develop an understanding of the states of stresses and strains in a Zirconia-yttria thermal barrier coating (TBC) experiencing a given temperature drop. Results so obtained are expected to facilitate experimental work. In order to gain realistic insights into the distribution of stresses and strains in a complex TBC, the finite element approach was selected to model a cylindrical TBC specimen. Experimental evidence reported in the literature indicated the presence of rough interface between the ceramic coat and bond coat. Oxidation of the bond coat at ceramic-bond interface was observed, as was a small amount of cracking in the ceramics near the ceramic-bond interface. To account for these complex features, a plane-strain finite element computer program known as TBCOC was developed, taking advantage of a generic computer code known as MARC. This generic code was made available through the use of a supercomputer (Cray 1). The TBCOC model contains 1316 nodal points and 2140 finite elements. It is capable of a uniform isothermal loading. Results of a sample computer run are presented.

Chang, G. C.↗

Joining of Silicon Carbide-Based Ceramics by Reaction Forming Method

Recently, there has been a surge of interest in the development and testing of silicon-based ceramics and composite components for a number of aerospace and ground based systems. The designs often require fabrication of complex shaped parts which can be quite expensive. One attractive way of achieving this goal is to build up complex shapes by joining together geometrically simple shapes. However, the joints should have good mechanical strength and environmental stability comparable to the bulk materials. These joints should also be able to maintain their structural integrity at high temperatures. In addition, the joining technique should be practical, reliable, and affordable. Thus, joining has been recognized as one of the enabling technologies for the successful utilization of silicon carbide based ceramic components in high temperature applications. Overviews of various joining techniques, i.e., mechanical fastening, adhesive bonding, welding, brazing, and soldering have been provided in recent publications. The majority of the techniques used today are based on the joining of monolithic ceramics with metals either by diffusion bonding, metal brazing, brazing with oxides and oxynitrides, or diffusion welding. These techniques need either very high temperatures for processing or hot pressing (high pressures). The joints produced by these techniques have different thermal expansion coefficients than the ceramic materials, which creates a stress concentration in the joint area. The use temperatures for these joints are around 700 C. Ceramic joint interlayers have been developed as a means of obtaining high temperature joints. These joint interlayers have been produced via pre-ceramic polymers, in-situ displacement reactions, and reaction bonding techniques. Joints produced by the pre-ceramic polymer approach exhibit a large amounts of porosity and poor mechanical properties. On the other hand, hot pressing or high pressures are needed for in-situ displacement reactions and reaction bonding techniques. Due to the equipment required, these techniques are impractical for joining large or complex shaped components.

Singh, M.↗

Silicon Carbide Fiber-Reinforced Silicon Nitride Composites

The fabrication and thermo-mechanical properties of SiC monofilament- and SiC fiber tow-reinforced reaction-bonded silicon nitride matrix composites (SiC/RBSN) and fully dense SiC monofilament-reinforced silicon nitride matrix composites (SiC/Si3N4) have been reviewed. The SiC/RBSN composites display high strength and toughness, and low thermal conductivity in the as-fabricated condition, but are susceptible to internal oxidation and mechanical property degradation in the intermediate temperature range from 400 to 1100 C. The internal oxidation problem can be avoided by applying functionally graded oxidation resistant coatings on external surfaces of the composite. On the other hand, the fully dense SiC/SiC3N4 composites fabricated by using SiC monofilaments and pressure assisted sintering methods display moderate strength and limited strain capability beyond matrix cracking stress. Advantages, disadvantages, and potential applications of SiC fiber-reinforced silicon nitride matrix composites fabricated using various fiber types and processing methods are discussed.

Bhatt, Ramakrishna T.↗

Fabrication of Microshutter Arrays for James Webb Space Telescope

Two-dimensional MEMS microshutter arrays are being developed at NASA Goddard Space Flight Center for use in the near-infrared region on the Next Generation Space Telescope (NGST). The microshutter arrays are designed for the selective transmission of light with high efficiency and high contrast. The NGST environment requires cryogenic operation at 45K. Microshutter arrays are fabricated out of silicon-oxide-insulated (SOI) silicon wafers. Arrays are close-packed silicon nitride membranes with a pixel size of 100x100 microns. Individual shutters are patterned with a torsion flexure permitting shutters to open 90 degrees with a minimized mechanical stress concentration. The mechanical shutter arrays are fabricated using MEMS technologies. The processing includes a multi-layer metal deposition and patterning of shutter electrodes and magnetic pads, reactive ion etching (RE) of the front side to form shutters out of the nitride membrane, an anisotropic back-etch for wafer thinning, followed by a deep RIE (DRIE) back-etch down to the nitride shutter membrane to form frames and relieve shutters from the silicon substrate. An additional metal deposition and patterning is used to form back electrodes. Shutters are actuated using a magnetic force and latched using an electrostatic force.

Li, Mary J.↗

Microshutter Arrays for James Webb Space Telescope

Two-dimensional MEMS microshutter arrays are being developed at NASA Goddard Space Flight Center for use in the near-infrared region on the James Webb Space Telescope (JWST). The microshutter arrays are designed for the selective transmission of light with high efficiency and high contrast. The JWST environment requires cryogenic operation at 35K. Microshutter arrays are fabricated out of silicon-oxide-insulated (SOI) silicon wafers. Arrays are close-packed silicon nitride membranes with a pixel size of 100x200 p. Individual shutters are patterned with a torsion flexure permitting shutters to open 90 degrees with a minimized mechanical stress concentration. The mechanical shutter arrays are fabricated using MEMS technologies. The processing includes a multi- layer metal deposition and patterning of shutter electrodes and magnetic pads, reactive ion etching (NE) of the front side to form shutters out of the nitride membrane, an anisotropic back-etch for wafer thinning, followed by a deep RIE (DRIE) back-etch down to the nitride shutter membrane to form W e s and relieve shutters from the silicon substrate. An additional metal deposition and patterning is used to form back electrodes. Shutters are actuated using a magnetic force and latched using an electrostatic force. . . . KEYWORDS: microshutter, MEMS, RIE, DRIE, micro-optics, near inbred, space telescope

Li, Mary J.↗

Programmable Aperture with MEMS Microshutter Arrays

A microshutter array (MSA) has been developed for use as an aperture array for multi-object selections in James Webb Space Telescope (JWST) technology. Light shields, molybdenum nitride (MoN) coating on shutters, and aluminum/aluminum oxide coatings on interior walls are put on each shutter for light leak prevention, and to enhance optical contrast. Individual shutters are patterned with a torsion flexure that permits shutters to open 90 deg. with a minimized mechanical stress concentration. The shutters are actuated magnetically, latched, and addressed electrostatically. Also, micromechanical features are tailored onto individual shutters to prevent stiction. An individual shutter consists of a torsion hinge, a shutter blade, a front electrode that is coated on the shutter blade, a backside electrode that is coated on the interior walls, and a magnetic cobalt-iron coating. The magnetic coating is patterned into stripes on microshutters so that shutters can respond to an external magnetic field for the magnetic actuation. A set of column electrodes is placed on top of shutters, and a set of row electrodes on sidewalls is underneath the shutters so that they can be electrostatically latched open. A linear permanent magnet is aligned with the shutter rows and is positioned above a flipped upside-down array, and sweeps across the array in a direction parallel to shutter columns. As the magnet sweeps across the array, sequential rows of shutters are rotated from their natural horizontal orientation to a vertical open position, where they approach vertical electrodes on the sidewalls. When the electrodes are biased with a sufficient electrostatic force to overcome the mechanical restoring force of torsion bars, shutters remain latched to vertical electrodes in their open state. When the bias is removed, or is insufficient, the shutters return to their horizontal, closed positions. To release a shutter, both the electrode on the shutter and the one on the back wall where the shutter sits are grounded. The shutters with one or both ungrounded electrodes are held open. Sub-micron bumps underneath light shields and silicon ribs on back walls are the two features to prevent stiction. These features ensure that the microshutter array functions properly in mechanical motions. The MSA technology can be used primarily in multi-object imaging and spectroscopy, photomask generation, light switches, and in the stepper equipment used to make integrated circuits and MEMS (microelectromechanical systems) devices.

Moseley, Samuel↗

Creating Hydride Rim Structures in Zircaloy 4 Cladding Tubes to Mimic High Burnup

During their long service in commercial light water reactors, zirconium alloy cladding tubes are subject to oxidation and subsequent hydrogen pickup which can degrade the materials mechanical properties [1]. These degradations can lead to premature cladding ruptures during reactor power transients [2] as well as negatively impact the claddings post quench ductility following high temperature steam oxidation in thermal hydraulic transients [3]. Hydrogen has low solid solubility in zirconium and usually precipitates as brittle zirconium hydride platelets in the cladding metal matrix. Due to temperature driven diffusion (Soret effect) and the grain texture of stress relieved zirconium metal tubes, these hydrides precipitate with a circumferential orientation near the outer surface of the cladding tubes forming a hydride rim which can serve as a site for crack initiation during circumferential ‘hoop’ loading of the cladding [4rim formation][5]. In order to better understand the effect of hydride rims on the fracture behavior of stress relieved zirconium alloy cladding tubes a procedure to produce these rim-like structures is being developed at Idaho National Laboratory (INL).

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Advanced Anode for Internal Reforming and Thermal Management in Solid Oxide Fuel Cells

Solid oxide fuel cell (SOFC) is an efficient and clean electrical power generation system compared to conventional combustion based technologies with energy efficiency reaching as high as 85-90% in co-generation mode (electricity and heat). Other advantages of SOFCs are hybridization, modularity of construction, small CO 2 foot print per kWh of generated electricity and fuel flexibility. Hydrocarbons present in the gaseous fuel is utilized in SOFCs by internal or external reforming. There are two different internal reforming concepts: Direct Internal Reforming (DIR) and Indirect Internal Reforming (IIR). For DIR operation, the endothermic reforming reaction and the exothermic reaction from the oxidation reaction are operated together in the single unit eliminating the requirement for a separate fuel reformer. This configuration also simplifies the overall system design, making SOFC more attractive and efficient means of producing electrical power. The main advantage of the DIR type of operation is that the H 2 or CO consumption by the electrochemical reaction could directly promote the conversion of methane at the anode side of the fuel cell resulting in high conversion and high efficiency. The DIR operation, however, requires an anode material that has desired dual catalytic (hetero and electro) properties for reforming reaction and electrochemical reactions. The anode materials also need to remain resistant to carbon formation at the operating temperature and atmosphere with stable cell performance. Another requirement is to match the reforming reactions and electrochemical reactions to avoid local cooling or overheating, which can result in mechanical failure due to thermally induced stresses. Direct internal reforming (DIR) of hydrocarbon fuels simplifies the overall SOFC system design making it more attractive and efficient for producing electrical power. Low cost alloy anodes for distributed internal reforming of methane and other hydrocarbon fuels offer increased fuel-flexibility, reliability, and long term performance stability of solid oxide fuel cells (SOFC). The research program examined modification of the chemical compositions and microstructure of high entropy alloy (HEA) anode materials using thermochemical calculations and process simulation and modeling to achieve distributed reforming over the entire anode to eliminate hot zones. Cell fabrication and testing of the HEA anodes using button cell configuration has been performed to demonstrate the advantages of new anode over traditional Ni-YSZ anodes for distributed reforming and carbon free operation. Technical accomplishments include identification and synthesis of HEA carbon-resistant anode, demonstration of reduction in reforming rate confirmed by GC and modelling data validating effectiveness for thermal management in cell/stacks, electrochemical testing of HEA anode in single cell (HEA-GDC||YSZ||LSM-YSZ) and Characterization of pretest and posttest anode materials by TEM and SEM-EDS confirming carbon-free operation.

30 DIRECT ENERGY CONVERSION↗

Strengthening of oxidation resistant materials for gas turbine applications

Compressive surface layers were formed on hot-pressed silicon carbide and nitride. The objective of these treatments was to improve the impact resistance of these materials at 1590 K (2400 F). Quenching was used to form compressive surface layers on silicon carbide. The presence of the compressive stresses was demonstrated by slotted rod tests. Compressive stresses were retained at elevated temperatures. Improvements in impact resistance at 1590 K (2400 F) and flexural strength at room temperature were achieved using cylindrical rods 3.3 mm (0.13 in.) in diameter. Carburizing treatments were used to form the surface layers on silicon nitride. In a few cases using rectangular bars improvements in impact resistance at 1590 K (2400 F) were observed.

Platts, D. R.↗