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At least 91 records · Page 5

Atomic-Scale Structure and Non-Stoichiometry of Meteoritic Hibonite: A Transmission Electron Microscope Study

Hibonite (CaAl_12O_19) is a common refractory mineral in Ca-Al-rich inclusions (CAIs) in primitive meteorites. Transmission electron microscope (TEM) studies have identified enigmatic planar defects in different occurrences of hibonite in the Allende meteorite that give rise to strong streaking along c* in electron diffraction patterns. Atomic resolution high-angle annular dark-field (HAADF) imaging and energy-dispersive X-ray (EDX) analyses were used to determine the nature and origin of these planar features. HAADF images of hibonite grains reveal lamellar intergrowths of common 1.6 nm spacing, and less commonly 2.0 and 2.5 nm spacings, interspersed in stoichiometric hibonite showing 1.1 nm (002) spacing. Stoichiometric hibonite consists of alternating Ca-containing (“R”) and spinel-structured (“S”) blocks stacked in a sequence RS. In contrast, the 1.6 nm layers result from a doubled S block such that the stacking sequence is RSS, while in the widest defect observed, the stacking sequence is RSSSS. These intergrowths are epitaxial and have coherent, low-strain boundaries with the host hibonite Meteoritic hibonite shows common Ti and Mg substitution for Al in its structure. Atomic-resolution EDX maps of hibonite grains in the Allende CAI confirm the preferred site occupancy of Mg on tetragonal M3 sites in S blocks and of Ti on trigonal bipyramidal M2 and octahedral M4 sites in R blocks. Mg is highly concentrated, but Ti is absent in the planar defects where wider S blocks show Al-rich compositions compared to stoichiometric MgAl_2O_4 spinel. Therefore, Mg likely played the major role in the formation and metastability of planar defects in hibonite. Electron energy loss spectroscopy data from the Ti L_2,3 edge show the presence of mixed Ti oxidation states with ~ 15–20% of Ti as Ti^(3+) in hibonite, suggesting a direct substitution of Ti^(3+) ↔ Al^(3+) in hibonite. The remaining ~ 80–85% of Ti is present as Ti^(4+) and corresponding EDX analyses are consistent with the well-known coupled substitution 2Al^(3+) ↔ Ti^(4+) + Mg^(2+) being the major mechanism for Ti and Mg substitution in hibonite. The formation of planar defects in hibonite occurred during high-temperature nebular condensation or melting/crystallization processes. The occurrence of non-stoichiometric hibonite in the Allende CAI deviates from the mineral formation sequence predicted from equilibrium condensation models. Overall, our atomic resolution TEM observations signify non-equilibrium, kinetic-controlled crystal growth during the high-temperature formation of refractory solids in the early solar nebula.

hibonite↗

Friction Stir Welding Development at NASA, Marshall Space Flight Center

Friction stir welding (FSW) is a solid state process that pan be used to join materials without melting. The process was invented by The Welding Institute (TWI), Cambridge, England. Friction stir welding exhibits several advantages over fusion welding in that it produces welds with fewer defects and higher joint efficiency and is capable of joining alloys that are generally considered non-weldable with a fusion weld process. In 1994, NASA-Marshall began collaborating with TWI to transform FSW from a laboratory curiosity to a viable metal joining process suitable for manufacturing hardware. While teamed with TWI, NASA-Marshall began its own FSW research and development effort to investigate possible aerospace applications for the FSW process. The work involved nearly all aspects of FSW development, including process modeling, scale-up issues, applications to advanced materials and development of tooling to use FSW on components of the Space Shuttle with particular emphasis on aluminum tanks. The friction stir welding process involves spinning a pin-tool at an appropriate speed, plunging it into the base metal pieces to be joined, and then translating it along the joint of the work pieces. In aluminum alloys the rotating speed typically ranges from 200 to 400 revolutions per minute and the translation speed is approximately two to five inches per minute. The pin-tool is inserted at a small lead angle from the axis normal to the work piece and requires significant loading along the axis of the tool. An anvil or reaction structure is required behind the welded material to react the load along the axis of the pin tool. The process requires no external heat input, filler material, protective shielding gas or inert atmosphere typical of fusion weld processes. The FSW solid-state weld process has resulted in aluminum welds with significantly higher strengths, higher joint efficiencies and fewer defects than fusion welds used to join similar alloys.

McGill, Preston↗

A computer program to perform flow and thermal analysis during pressurization of the Space Shuttle Solid Rocket Motor field joint

A computational technique for prediction of the flow and thermal environment in the SRM field joint cavities is described. The SRM field joint hardware was tested with a defect in the insulation, and due to this defect, the O-ring gland cavities are pressurized during the early part of the ignition. A computer model is developed to predict the thermal environment and flow through the simulated flaw, during the pressurization of the field joint. The transient mass, momentum, and energy conservation equations in the flow passage together with the thermodynamic equation of state are solved by a fully implicit iterative numerical procedure.

Clayton, J. Louie↗

Shear strength of fillet welds in aluminum alloy 2219

Fillet size is discussed in terms of theoretical or design dimensions versus as-welded dimensions, drawing attention to the inherent conservatism in the design load sustaining capabilities of fillet welds. Emphasis is placed on components for the solid rocket motor, external tank, and other aerospace applications. Problems associated with inspection of fillet welds are addresses and a comparison is drawn between defect counts obtained by radiographic inspection and by visual examination of the fracture plane. Fillet weld quality is related linearly to ultimate shear strength. Correlation coefficients are obtained by simple straight line regression analysis between the variables of ultimate shear strength and accumulative discontinuity summation. Shear strength allowables are found to be equivalent to 57 percent of butt weld A allowables (F sub tu.)

Lovoy, C. V.↗

Ultrasonic Inspection Of Thick Sections

Ultrasonics used to inspect large, relatively thick vessels for hidden defects. Report based on experiments in through-the-thickness transmission of ultrasonic waves in both steel and filament-wound composite cases of solid-fuel rocket motors.

Friant, C. L.↗

Growth of mercuric iodide (HgI2) for nuclear radiation detectors

Mercuric iodide is a material used for the fabrication of the sensing element in solid state X-ray and gamma ray detecting instruments. The operation of the devices is determined to a large degree by the density of structural defects in the single crystalline material used in the sensing element. Since there were strong indications that the quality of the material was degraded by the effects of gravity during the growth process, a research and engineering program was initiated to grow one or more crystals of mercuric iodide in the reduced gravity environment of space. A special furnace assembly was designed which could be accommodated in a Spacelab rack, and at the same time made it possible to use the same growth procedures and controls used when growing a crystal on the ground. The space crystal, after the flight, was subjected to the same evaluation methods used for earth-grown crystals, so that comparisons could be made.

Vandenberg, L.↗

Unraveling the Material Processing Conditions for Optimizing FSW Process

In friction stir welding (FSW), a rotating threaded pin tool is inserted into a weld seam and literally stirs the edges of the seam together. This environmentally friendly, solid-state technique has been successfully used in the joining of materials that are difficult to fusion weld. To determine optimal processing parameters for producing a defect free weld a better understanding of the resulting metal deformation flow path and velocity is required. In this study the metal flow fields are marked by the use of thin (0.001? tungsten) wires embedded in the weld seam at various locations. X-ray radiographs record the position and segmentation of the wire and are used to elucidate the flow field. Microstructures observed in a FSW cross-section in an aluminum alloy are related to their respective strain-strain rate-temperature histories along their respective flow trajectories. Two kinds of trajectories, each subjecting the weld metal to a distinct thermomechanical process and imparting a distinct microstructure, can be differentiated within the weld structure.

Schneider, Judy↗

Quantifying the Material Processing Conditions for an Optimized FSW Process

In friction stir welding (FSW), a rotating threaded pin tool is inserted into a weld seam and literally stirs the edgs of the seam together. This environmentally friendly, solid-state technique has been successfully used in the joining of materials that are difficult to fusion weld. To determine optimal processing parameters for producing a defect free weld, a better understanding of the resulting metal deformation flow path and velocity is required. In this study the metal flow fields are marked by the use of thin (0.001 in. tungsten) wires embedded in the weld seam at various locations. X-ray radiographs record the position and segmentation of the wire and are used to elucidate the flow field. Microstructures observed in a FSW cross-section in an aluminum alloy are related to their respective strain-strain rate-temperature histones along their respective flow trajectories. Two kinds of trajectories, each subjecting the weld metal to a distinct thermomechanical process and imparting a distinct microstructure, can be differentiated within the weld structure.

Schneider, Judy↗

Bulk Crystal Growth of Piezoelectric PMN-PT Crystals Using Gradient Freeze Technique for Improved SHM Sensors

There has been a growing interest in recent years in lead based perovskite ferroelectric and relaxor ferroelectric solid solutions because of their excellent dielectric, piezoelectric and electrostrictive properties that make them very attractive for various sensing, actuating and structural health monitoring (SHM) applications. We are interested in the development of highly sensitive and efficient PMN-PT sensors based on large single crystals for the structural health monitoring of composite materials that may be used in future spacecrafts. Highly sensitive sensors are needed for detection of defects in these materials because they often tend to fail by distributed and interacting damage modes and much of the damage occurs beneath the top surface of the laminate and not detectable by visual inspection. Research is being carried out for various combinations of solid solutions for PMN-PT piezoelectric materials and bigger size crystals are being sought for improved sensor applications. Single crystals of this material are of interest for sensor applications because of their high piezoelectric coefficient (d33 greater than 1700 pC/N) and electromechanical coefficients (k33 greater than 0.90). For comparison, the commonly used piezoelectric ceramic lead zirconate titanate (PZT) has a d33 of about 600 pC/N and electromechanical coefficients k33 of about 0.75. At the present time, these piezoelectric relaxor crystals are grown by high temperature flux growth method and the size of these crystals are rather small (~3x4x5 mm(exp 3). In the present paper, we have attempted to grow bulk single crystals of PMN-PT in a 2 inch diameter platinum crucible and successfully grown a large size crystal of 67%PMN-33%PT using the vertical gradient freeze technique with no flux. Piezoelectric properties of the grown crystals are investigated. PMN-PT plates show excellent piezoelectric properties. Samples were poled under an applied electric field of 5 kV/cm. Dielectric properties at a frequency of 1 kHz are examined. The grown PMN-PT crystals show typical relaxor dielectric properties. Additionally, the thermal properties of the sample are tested. The results are in good agreement with those found in the literature and some are reported for the first time.

Aggarwal, Mohan D.↗

Complex Intergrowths of Non-Stoichiometric Defect-Structured Hibonite and Al-Rich Spinel in an Allende Ca-Al-Rich Inclusion

Hibonite is a primary ultra-refractory mineral occurring in many Ca-Al-rich inclusions (CAIs) and is predicted to condense as the second major phase from a cooling gas of solar composition. Our previous microstructural studies of hibonite in carbonaceous chondrites revealed its unique microstructures consisting of numerous defects that contain Mg-enriched, wider spinel blocks in stoichiometric hibonite. Han, J. et al. [2 items] demonstrated experimentally that defect-structured hibonites can grow easily in the presence of minor Mg and are kinetically more stable than equilibrium assemblages predicted by thermodynamic calculations. However, a thermo-dynamic vs. structural stability of defect-structured hibonite relative to other early-condensed Al-rich phases such as corundum, grossite, and spinel remains poorly constrained. Here, we present the results of atomic resolution TEM (Transmission Electron Microscopy) imaging of hibonite in a compact Type A CAI in the Allende CV3 chondrite in order to better understand the crystal structure and chemistry of defect-structured hibonite and its associated Al-rich phases, especially non-stoichiometric, Al-rich spinel, in the context of the formation of first refractory solids in the early solar nebula.

Han, J.↗

Computer Tomography 3-D Imaging of the Metal Deformation Flow Path in Friction Stir Welding

In friction stir welding, a rotating threaded pin tool is inserted into a weld seam and literally stirs the edges of the seam together. This solid-state technique has been successfully used in the joining of materials that are difficult to fusion weld such as aluminum alloys. To determine optimal processing parameters for producing a defect free weld, a better understanding of the resulting metal deformation flow path is required. Marker studies are the principal method of studying the metal deformation flow path around the FSW pin tool. In our study, we have used computed tomography (CT) scans to reveal the flow pattern of a lead wire embedded in a FSW weld seam. At the welding temperature of aluminum, the lead becomes molten and thus tracks the aluminum deformation flow paths in a unique 3-dimensional manner. CT scanning is a convenient and comprehensive way of collecting and displaying tracer data. It marks an advance over previous more tedious and ambiguous radiographic/metallographic data collection methods.

Schneider, Judy↗

Analysis of Composite Panel-Stiffener Debonding Using a Shell/3D Modeling Technique

Interlaminar fracture mechanics has proven useful for characterizing the onset of delaminations in composites and has been used successfully primarily to investigate onset in fracture toughness specimens and laboratory size coupon type specimens. Future acceptance of the methodology by industry and certification authorities, however, requires the successful demonstration of the methodology on the structural level. For this purpose, a panel was selected that is reinforced with stiffeners. Shear loading causes the panel to buckle, and the resulting out-of-plane deformations initiate skin/stiffener separation at the location of an embedded defect. A small section of the stiffener foot, web and noodle as well as the panel skin in the vicinity of the delamination front were modeled with a local 3D solid model. Across the width of the stiffener foot, the mixedmode strain energy release rates were calculated using the virtual crack closure technique. A failure index was calculated by correlating the results with a mixed-mode failure criterion of the graphite/epoxy material. Computed failure indices were compared to corresponding results where the entire web was modeled with shell elements and only a small section of the stiffener foot and panel were modeled locally with solid elements. Including the stiffener web in the local 3D solid model increased the computed failure index. Further including the noodle and transition radius in the local 3D solid model changed the local distribution across the width. The magnitude of the failure index decreased with increasing transition radius and noodle area. For the transition radii modeled, the material properties used for the noodle area had a negligible effect on the results. The results of this study are intended to be used as a guide for conducting finite element and fracture mechanics analyses of delamination and debonding in complex structures such as integrally stiffened panels.

Krueger, Ronald↗

Scintillation Breakdowns in Chip Tantalum Capacitors

Scintillations in solid tantalum capacitors are momentarily local breakdowns terminated by a self-healing or conversion to a high-resistive state of the manganese oxide cathode. This conversion effectively caps the defective area of the tantalum pentoxide dielectric and prevents short-circuit failures. Typically, this type of breakdown has no immediate catastrophic consequences and is often considered as nuisance rather than a failure. Scintillation breakdowns likely do not affect failures of parts under surge current conditions, and so-called "proofing" of tantalum chip capacitors, which is a controllable exposure of the part after soldering to voltages slightly higher than the operating voltage to verify that possible scintillations are self-healed, has been shown to improve the quality of the parts. However, no in-depth studies of the effect of scintillations on reliability of tantalum capacitors have been performed so far. KEMET is using scintillation breakdown testing as a tool for assessing process improvements and to compare quality of different manufacturing lots. Nevertheless, the relationship between failures and scintillation breakdowns is not clear, and this test is not considered as suitable for lot acceptance testing. In this work, scintillation breakdowns in different military-graded and commercial tantalum capacitors were characterized and related to the rated voltages and to life test failures. A model for assessment of times to failure, based on distributions of breakdown voltages, and accelerating factors of life testing are discussed.

Teverovsky, Alexander↗

Thermal Barriers Developed for Solid Rocket Motor Nozzle Joints

Space shuttle solid rocket motor case assembly joints are sealed with conventional O-ring seals that are shielded from 5500 F combustion gases by thick layers of insulation and by special joint-fill compounds that fill assembly splitlines in the insulation. On a number of occasions, NASA has observed hot gas penetration through defects in the joint-fill compound of several of the rocket nozzle assembly joints. In the current nozzle-to-case joint, NASA has observed penetration of hot combustion gases through the joint-fill compound to the inboard wiper O-ring in one out of seven motors. Although this condition does not threaten motor safety, evidence of hot gas penetration to the wiper O-ring results in extensive reviews before resuming flight. The solid rocket motor manufacturer (Thiokol) approached the NASA Glenn Research Center at Lewis Field about the possibility of applying Glenn's braided fiber preform seal as a thermal barrier to protect the O-ring seals. Glenn and Thiokol are working to improve the nozzle-to-case joint design by implementing a more reliable J-leg design and by using a braided carbon fiber thermal barrier that would resist any hot gases that the J-leg does not block.

Steinetz, Bruce M.↗

Growth of Solid Solution Single Crystals

The solidification of a solid solution semiconductor, having a wide separation between liquidus and serious has been extensively studied in ground based, high magnetic field and Spacelab experiments. Two alloys of mercury cadmium telluride have been studied; mercury cadmium telluride with 80.0 mole percent of HgTe and 84.8 mole percent respectively. These alloys are extremely difficult to grow by directional solidification on earth due to high solutal and thermal density differences that give rise to fluid flow and consequent loss of interface shape and composition. Diffusion controlled growth is therefore impossible to achieve in conventional directional solidification. The ground based experiments consisted of growing crystals in several different configurations of heat pipe furnaces, NASA's Advanced Automated Directional Solidification Furnace (AADSF), and a similar furnace incorporated in a superconducting magnet capable of operating at up to 5T. The first microgravity experiment took place during the flight of STS-62 in March 1994, with the AADSF installed on the second United States Microgravity Payload (USMP-2). The alloy was solidified at 3/4 inch per day over a 9 day period, and for the first time a detailed evaluation was performed of residual acceleration effects. The second flight experiment took place in the fourth United States Microgravity Payload Mission (USMP-4) in November 1997. Due to contamination of the furnace system by a previously processed sample, the sample was not received until May 1998, and the preliminary analysis shows that the conditions prevailing during the experiment were quite different from the requirements requested prior to the mission. Early results are indicating that the sample may not accomplish the desired objectives. As with the USMP-2 mission, the results of the ground based experiments were compared with the crystal grown in orbit under microgravity conditions. On the earth, it has been demonstrated that the application of the magnetic field leads to a significant reduction in fluid flow, with improved homogeneity of composition. The field strength required to suppress flow increases with diameter of the material. The 8 mm diameter sample used here was less than the upper diameter limit for a ST magnet. The configuration for USMP-4 was changed so that the material was seeded and other processing techniques were also modified. It was decided to examine the effects of a strong magnetic field under the modified configuration and parameters. A further change from USMP-2 was that a different composition of material was grown, namely with 0.152 mole fraction of cadmium telluride rather than the 0.200 of the USMP-2 experiment. The objective was to grow highly homogeneous, low defect density material of a composition at which the conduction band and the valence band of the material impinge against each other. As indicated, the furnace was contaminated during the mission. As a result of solid debris remaining in the furnace bore, the cartridge in this experiment, denoted as SL1-417, was significantly bent during the insertion phase. During translation the cartridge scraped against the plate which isolates the hot and cold zones of the furnace. Thermocouples indicated that a thermal assymetry resulted. The scraping in the slow translation or crystal growth part of the processing was not smooth and it is probable that the jitter was sufficient to give rise to convection in the melt. Early measurements of composition from the surface of the sample have shown that the composition varies in an oscillatory manner.

Lehoczky, Sandor L.↗

Flight service evaluation of Kevlar-49/epoxy composite panels in wide-bodied commercial transport aircraft

Kevlar-49 fairing panels were inspected and found to be performing satisfactorily after two years flight service on an Eastern and an Air Canada L-1011. Six panels are on each aircraft including sandwich and solid laminate wing-body panels, and 300 F service aft engine fairings. Some of the panels were removed from the aircraft to permit inspection of inner surfaces and fastener hole conditions. Minor defects such as surface cracks due to impact damage, small delaminated areas, elongation and fraying of fastener holes, were noted. None of these defects were considered serious enough to warrant corrective action in the opinion of airline personnel. The defects are typical for the most part of defects noted on similar fiberglass parts.

Stone, R. H.↗