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NASA NTRS1993

Room temperature degradation of YBa2Cu3O(7-x) superconductors in varying relative humidity environments

An aging study was performed to determine the stability of YBa2Cu3O(7-x) ceramics in humid environments at 20 C. In this study, fired ceramic specimens were exposed to humidity levels ranging from 30.5 to 100 percent for 2-, 4-, and 6-week time intervals. After storage under these conditions, the specimens were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), and electrical resistance measurements. At every storage condition evaluated, the fired ceramics were found to interact with H2O present in the surrounding environment, resulting in the decomposition of the YBa2Cu3O(7-x) phase. XRD data showed that BaCO3, CuO, and Y2BaCuO5 were present after aging and that the peak intensities of these impurity phases increased both with increasing humidity level and with increasing time of exposure. Additionally, SEM analyses of the ceramic microstructures after aging revealed the development of needle-like crystallites along the surface of the test specimens after aging. Furthermore, the superconducting transition temperature T(sub c) was found to decrease both with increasing humidity level and with increasing time of exposure. All the specimens aged at 30.5, 66, and 81 percent relative humidity exhibited superconducting transitions above 80 K, although these values were reduced by the exposure to the test conditions. Conversely, the specimens stored in direct contact with water (100 percent relative humidity) exhibited no superconducting transitions.

Hooker, M. W.↗
NASA NTRS1993

Surface characterization of LDEF materials

The NASA Long Duration Exposure Facility (LDEF), a passive experimental satellite, was placed into low-Earth orbit by the Shuttle Challenger in Apr. 1984. The LDEF spent an unprecedented 69 months in space. The flight and recovery of the LDEF provided a wealth of information on the longterm space environmental effects of a variety of materials exposed to the low-Earth orbit environment. Surface characterization of LDEF materials included polymers, composites, thermal control paints, and aluminum. X-ray photoelectron spectroscopy (XPS), Auger electron spectroscopy (AES), scanning electron microscopy (SEM), and contact angle analysis were used to document changes in both the surface composition and surface chemistry of these materials. Detailed XPS analysis of the polymer systems, such as Kapton, polyimide polysiloxane copolymers, and fluorinated ethylene propylene thermal blankets on the backside of the LDEF revealed significant changes in both the surface composition and surface chemistry as a result of exposure to the low-Earth orbit environment. Polymer systems such as Kapton, polyimide polysiloxane copolymers, and polysulfone showed a common trend of decreasing carbon content and increasing oxygen content with respect to the control sample. Carbon 1s curve fit XPS analysis of the composite samples, in conjunction with SEM photomicrographs, revealed significant ablation of the polymer matrix resin to expose the carbon fibers of the composite during exposure to the space environment. Surface characterization of anodized aluminum tray clamps, which were located at regular intervals over the entire LDEF frame, provided the first results to evaluate the extent of contamination with respect to position on the LDEF. The XPS results clearly showed that the amount and state of both silicon and fluorine contamination were directly dependent upon the position of the tray clamp on the LDEF.

Wightman, J. P.↗
NASA NTRS1993

Heterogeneous plagioclase compositions in the Maralinga CK4 chondrite

One of the characteristic features of CK chondrites is the wide compositional range displayed by feldspar grains in matrix relative to the narrow range of compositions exhibited by the highly equilibrated olivines and pyroxenes. Recently, it was suggested that these heterogeneous feldspar compositions may have been strongly influenced by shock metamorphisms. It is shown that the apparent range of feldspar compositions in Maralinga probably results from annealing during parent body thermal metamorphism rather than shock. The majority of matrix feldspars in Maralinga are typically 50 microns in size and are compositionally zoned, with oligoclase cores (approximately An40) and bytownite rims (approximately An80). The contact between core and rim is sharp and abrupt and is readily observed in backscattered scanning electron microscopy (SEM) images.

Keller, Lindsay P.↗
NASA NTRS1993

Carbon abundances, major element chemistry, and mineralogy of hydrated interplanetary dust particles

Hydrated interplanetary dust particles (IDP's) comprise a major fraction of the interplanetary dust particles collected in the stratosphere. While much is known about the mineralogy and chemistry of hydrated IDP's, little is known about the C abundance in this class of IDP's, the nature of the C-bearing phases, and how the C abundance is related to other physical properties of hydrated IDP's. Bulk compositional data (including C and O) for 11 hydrated IDP's that were subsequently examined by the transition electron microscopy (TEM) to determine their mineralogy and mineral chemistry are reported. Our analysis indicates that these hydrated IDP's are strongly enriched in C relative to the most C-rich meteorites. The average abundance of C in these hydrated IDP's is 4X CI chondrite values. The bulk compositions (including C and O) of 11 hydrated IDP's were determined by thin-window, energy-dispersive x ray (EDX) spectroscopy of the uncoated IDP's on Be substrates in the scanning electron microscopy (SEM). As a check on our C measurements, one of the IDP's (L2006H5) was embedded in glassy S, and microtome thin sections were prepared and placed onto Be substrates. Thin-film EDX analyses of multiple thin sections of L2006H5 show good agreement with the bulk value determined in the SEM. Following EDX analysis, the mineralogy and mineral chemistry of each IDP was determined by analyzing ultramicrotome thin sections in a TEM equipped with an EDX spectrometer.

Keller, L. P.↗
NASA NTRS1993

New technique for oil backstreaming contamination measurements

Due to the large size and the number of diffusion pumps, space simulation chambers cannot be easily calibrated by the usual test dome method for measuring backstreaming from oil diffusion pumps. In addition, location dependent contamination may be an important parameter of the test. The backstreaming contamination in the Space Power Facility (SPF) near Sandusky, Ohio, the largest space simulation vacuum test chamber in the U.S.A. was measured. Small size clean silicon wafers as contamination sensors placed at all desired measurement sites were used. The facility used diffusion pumps with DC 705 oil. The thickness of the contamination oil film was measured using ellipsometry. Since the oil did not wet uniformly the silicon substrate, two analysis models were developed to measure the oil film: continuous, homogeneous film and islands of oil with the islands varying in coverage fraction and height. In both cases, the contamination film refractive index was assumed to be that of DC 705. The second model improved the ellipsometric analysis quality parameter by up to two orders of magnitude, especially for the low coverage cases. Comparison of the two models for our case shows that the continuous film model overestimates the oil volume by less than 50 percent. Absolute numbers for backstreaming are in good agreement with published results for diffusion pumps. Good agreement was also found between the ellipsometric results and measurements done by x ray photoelectron spectroscopy (XPS) and by scanning electron microscopy (SEM) on samples exposed to the same vacuum runs.

Alterovitz, S. A.↗
NASA NTRS1994

Shape, size, and distribution of magnetic particles in Bjurbole chondrules

Chondrules from the Bjurbole chondritic meteorite (L4) exhibit saturation remanence magnetization (SIRM) values which vary over three orders of magnitude. REM values (Natural Remanence Magnetization/SIRM) for Allende (C3V) and Chainpur (LL3) are less than 0.01 but in Bjurbole some chondrules were found to have REM values greater than 0.1 with several greater than 0.2. REM values greater than 0.1 are abnormal and cannot be acquired during weak field cooling. If exposure to a strong field (whatever the source) during the chondrules' history is responsible for the high REM values, was such history associated with a different processing which might have resulted in different shape, size, and distribution of metal particles compared to chondrules having REM values of less than 0.01? Furthermore, magnetic hysteresis results show a broad range of magnetic hardness and other intrinsic magnetic properties. These features must be related to (1) size and amount of metal; and (2) properties of, and amount of, tetrataenite in the chondrules (all chondrules thus far subjected to thermomagnetic analysis show the presence of tetrataenite). A scanning electron microscopy (SEM) study is underway to determine the relationship between the shape, size, and distribution of metal particles within individual chondrules and the magnetic properties of these chondrules. Results from the SEM study in conjunction with magnetic property data may also help to discern effects from possible lightning strikes in the nebula prior to incorporation of the chondrules into the parent body.

Nava, David F.↗
NASA NTRS1993

Burn rates of TiH2/KClO4/Viton and output testing of NASA SKD26100098-301 pressure cartridges

The burn rates of the pyrotechnic TiH2/KClO4/Viton with a mass ratio of 30/65/5 have been measured as a function of pressure in nitrogen up to 312 MPa(45 Kpsi). The burn rates were fit to R = a pn, with a = 2.055 cm/sec/MPan and n = 0.472 between 0.15 MPa (22 psi) and 21.6 MPa (3.13 Kpsi) and a = 4.38 cm/sec/MPan and n = 0.266 between 70 MPa (10.15 Kpsi) and 312 MPa (45.25 Kpsi). The decrease in slope at the higher pressures is attributed to a diffusion limited reaction. No acoustically driven flame instabilities or large conductive-to-convective burn transitions were observed. Solid reaction products were analyzed by x-ray diffraction and scanning electron microscopy (SEM). X-ray diffraction detected only TiO2 and KC1. SEM showed that the particle size of the reaction products increased as the nitrogen pressure increased. There were no anomalous characteristics of the burn of this pyrotechnic that could be interpreted as a cause of the o-ring blow-by problem in the forward shear bolt assembly. Three NASA SKD26100098-301 pressure cartridges were fired into a fixed volume vessel that was sealed with an O-ring. A maximum pressure of 181.7 MPa(26,350 psi) was reached in around 100 ,mu sec for two shots fired into a volume of 16.3 cm3(0.996 in3). A maximum pressure of 33,460 psi was reached for one shot fired into a volume of 9.55 cm3(0.583 in3). The O-ring burned through on one shot in the larger volume and leaked on the other two thereby simulating the effects of an O-ring leak. The results imply that the piston in the shear bolt assembly would receive a large impulse even if there was a leak in an O-ring seal.

Holy, John A.↗
NASA NTRS1994

Textural variability of ordinary chondrite chondrules: Implications of their formation

Scanning electron microscopy (SEM) and microprobe examination of the Raguli H3-4, Saratov L3, and Fucbin L5-6 ordinary chondrites and the analysis of preexisted data on other meteorites have shown that the variety of textural types of chondrules depends on the chemical composition of the chondrules. The comparison of bulk-rock chemistries of the chondrules by major components demonstrates that they apparently fall, like basic-ultrabasic rock, into groups of dunitic and pyroxenitic composition. This separation is further validated by the character of zoning in chondrules of the intermediate, peridotitic type. The effect is vividly demonstrated by the 'chondrule-in-chondrule' structure.

Zinovieva, N. G.↗
NASA NTRS1995

Natural and orbital debris particles on LDEF's trailing and forward-facing surfaces

Approximately 1000 impact craters on the Chemistry of Meteoroid Experiment (CME) have been analyzed by means of Scanning Electron Microscopy (SEM) and Energy Dispersive X-ray Analysis (EDXA) to determine the compositional make-up of projectile residues. This report completes our systematic survey of gold and aluminum surfaces exposed at the trailing-edge (A03) and forward-facing (A11) LDEF sites, respectively. The major categories for the projectile residues were (1) natural, with diverse subgroups such as chondritic, monomineralic silicates, and sulfides, and (2) man made, that were classified into aluminum (metallic or oxide) and miscellaneous materials (such as stainless steel, paint flakes, etc). On CME gold collectors on LDEF's trailing edge approximately 11 percent of all craters greater than 100 micron in diameter were due to man-made debris, the majority (8.6 percent) caused by pure aluminum, approximately 31.4 percent were due to cosmic dust, while the remaining 58 percent were indeterminate via the analytical techniques utilized in this study. The aluminum surfaces located at the A11 forward-facing site did not permit analysis of aluminum impactors, but approximately 9.4 percent of all craters were demonstratably caused by miscellaneous debris materials and approximately 39.2 percent were the result of natural particles, leaving approximately 50 percent which were indeterminate. Model considerations and calculations are presented that focus on the crater-production rates for features greater than 100 micron in diameter, and on assigning the intermediate crater population to man-made or natural particles. An enhancement factor of 6 in the crater-production rate of natural impactors for the 'forward-facing' versus the 'trailing-edge' CME collectors was found to best explain all observations (i.e., total crater number(s), as well as their computational characteristics). Enhancement factors of 10 and 4 are either too high or too low. It is also suggested that approximately 45 percent of all craters greater than 100 micron in diameter are caused by man-made impactors on the A11 surfaces. This makes the production rate for craters greater than 100 micron in diameter, resulting from orbital debris, a factor of 40 higher on the forward-facing sides as opposed to the trailing-edge direction.

Hoerz, Friedrich↗
NASA NTRS1994

Aubrite basalt vitrophyres: High sulfur silicate melts and a snapshot of aubrite formation

Two aubrite basalt vitrophyre clasts have been found within AMNH thin sections from the Parsa EH3 chondrite and the Khor Temiki aubrite. Polished sections of the Parsa Aubrite Inclusion (PAI) and the Khor Temiki Inclusion (KTI) were studied by optical, electron probe microanalysis (EPMA), and scanning electron microscopy (SEM) techniques with broad-beam and low absorbed EPMA currents used to minimize glass volatile loss. Some data have previously been reported for PAI and KTI may possibly correlate to a previously reported inclusion in Khor Tiimiki. In polished sections, PAI and KTI are approximately equal 4 mm in diameter and contain a large volume of glass. The clasts have similar textural characteristics and are akin to lunar vitrophyre textures. The glasses have high alkali rhyodacitic compositions Al-though PAI is peraluminous, KTI is significantly peralkaline. Additionally, the glasses have elevated sulfur concentrations that are extremely high by geochemical standards. SEM examination for beam overlap of microscopic CaS, FeS, and (Mg, Mn, Fe) S inclusions showed no such contamination. Furthermore, homogeneity of glass S content and low FeO contents help rule out contamination. Materials research data show that under reducing conditions alumino-silicate melts can dissolve up to several weight percent sulfur in the absence of Fe. The high S and alkali contents, the lack of associated high shock features, and the rationalized phase equilibria suggest that PAI and KTI are igneous melting products of an E-chondrite-like source material. Although large-scale impact melting cannot totally be ruled out, the above observations eliminate the possibility of in-situ shock melting.

Fogel, R. A.↗
NASA NTRS1994

Mn-Cr isotopic systematics of individual Chainpur chondrules

Twenty-eight chondrules separated from Chainpur (LL3.4) were surveyed for abundances of Mn, Cr, Na, Fe, Sc, Hf, Ir, and Zn by Instrumental Neutron Activation Analysis (INAA). Six, weighting 0.6-1.5 mg each, were chosen for Scanning Electron Microscopy (SEM)/Energy Dispersive X-ray (EDX) and high-precision Ce-isotopic studies. LL-chondrite-normalized (Mn/Fe)(sub LL) and (Sc/Fe)(sub LL) were found to be useful in categorizing them. Five chondrules (CH-16, -17, -18, -23, and -28) were in the range 0.5 less than (Mn/Fe)(sub LL) less than 1. 4 and 0.5 less than (Sc/Fe)(sub LL) less than 1.4. The sixth (CH-25) had (Mn/Fe)(sub LL) and (Sc/Fe)(sub LL) ratios of 0.40 and 8.1, respectively, and was enriched in the refractory lithophile elements Sc and Hf and the refractory siderophile element Ir by 2.7 and 4.4x LL abundances respectively. SEM/EDX of exterior surfaces of the chondrules showed they consisted of varying proportions of low- and high-Ca pyroxenes, olivine, glass, kamacite/taenite, and Fe-sulfides. Chromium-53/chromium-52 for the six chondrules and bulk Chainpur (WR) are presented. Chromium-54/chromium-52 is close to terrestrial and does not correlate with Mn/Cr. We provisionally ignore the possibility of initial Cr isotopic heterogeneities among the chondrules. Omitting both the CH-25 and WR data, a linear regression gives initial (Mn-53/Mn-55)(sub I) = 8 +/- 4 x 10(exp -6), corresponding to chondrule formation at Delta(t)(sub LEW) = -9 +/- 4 Ma prior to igneous crystallization of the LEW 86010 angrite. If initial (Mn-53/Mn-55)(sub 0) in the solar system were as high as approximately 4.4 x 10(exp -5) when Allende CAI formed, our data suggest Chainpur chondrules formed approximately 9 Ma later, in qualitative agreement with 'late' I-Xe formation ages for most Chainpur chondrules.

Nyquist, L.↗
NASA NTRS1994

An ion microprobe study of CAIs from CO3 meteorites

When attempting to interpret the history of Ca, Al-rich inclusions (CAIs) it is often difficult to distinguish between primary features inherited from the nebula and those produced during secondary processing on the parent body. We have undertaken a systematic study of CAIs from 10 CO chondrites, believed to represent a metamorphic sequence with the goal of distinguishing primary and secondary features. ALHA 77307 (3.0), Colony (3.0), Kainsaz (3.1), Felix (3.2), ALH 82101 (3.3), Ornans (3.3), Lance (3.4), ALHA 77003 (3.5), Warrenton (3.6), and Isna (3.7) were examined by Scanning Electron Microscopy (SEM) and optical microscopy. We have identified 141 CAIs within these samples, and studied in detail the petrology of 34 inclusions. The primary phases in the lower petrologic types are spinel, melilite, and hibonite. Perovskite, FeS, ilmenite, anorthite, kirschsteinite, and metallic Fe are present as minor phases. Melilite becomes less abundant in higher petrologic types and was not detected in chondrites of type 3.5 and above, confirming previous reports that this mineral easily breaks down during heating. Iron, an element that would not be expected to condense at high temperatures, has a lower abundance in spinel from low-petrologic-type meteorites than those of higher grade, and CaTiO3 is replaced by FeTiO3 in meteorites of higher petrologic type. The abundance of CAIs is similar in each meteorite. Eight inclusions have been analyzed by ion probe. The results are summarized. The results obtained to date show that CAIs in CO meteorites, like those from other meteorite classes, contain Mg* and that Mg in some inclusions has been redistributed.

Russell, S. S.↗
NASA NTRS1995

Nullarbor 018: A new L6 chondrite from Australia

A new meteorite find from the Nullarbor Plain in Australia was studied using optical, scanning electron microscopy (SEM), and electron microprobe techniques. The meteorite, Nullarbor 018, is an orthodox L6 chondrite that experienced minor-to-moderate alteration of metal during terrestrial weathering (grade A-B to B). During weathering, trolite was preferentially altered, and roughly 20% of the original complement of S in the meteorite was removed. Shock metamorphic effects corresponding to shock stage S4 (or shock facies d) are found, including the presence of some diaplectic feldspar (maskelynite). The meteorite is not obviously paired with other finds from the Nullarbor region, but the possibility that it is paired cannot be excluded.

Ruzicka, Alex↗
NASA NTRS1995

Improvement of critical current density in thallium-based (Tl,Bi)Sr(1.6)Ba(0.4)Ca2Cu3O(x) superconductors

Epitaxial (Tl,Bi)Sr(1.6)Ba(0.4)Ca2Cu3O(x) ((Tl,Bi)-1223) thin films on (100) single crystal LaAlO3 substrates were synthesized by a two-step procedure. Phase development, microstructure, and relationships between film and substrate were studied by X-ray diffraction (XRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). Resistance versus temperature, zero-field-cooled and field cooled magnetization, and transport critical current density (J(sub c)) were measured. The zero-resistance temperature was 105-111 K. J(sub c) at 77 K and zero field was greater than 2 x 10(exp 6) A/sq cm. The films exhibited good flux pinning properties.

Ren, Z. F.↗
NASA NTRS1995

An investigation of the loss of ductility in hydrogen charged beta-Ti alloys

The high strength, low density, and good corrosion resistance of Ti-based alloys make them candidate materials for a number of applications in the aerospace industry. A major limitation in the use of these alloys in the advanced hypersonic flight vehicle program is their susceptibility to hydrogen embrittlement. This study focuses on the hydrogen sensitivity of TIMETAL 21S beta-Ti alloy. The material received was in the form of grip-ends of failed tensile test samples which had been exposed to different charging conditions (combinations of hydrogen pressure and temperature). The samples received, the charging conditions, and their fracture mode are discussed. It can be seen that the fracture behavior changes from ductile to brittle with increasing hydrogen content, but the transition in behavior occurs for a small increase in hydrogen concentration. The aim of this program was to assess the microstructural differences between the ductile and brittle alloys to ascertain the embrittlement mechanism. A range of tools which included x-ray diffraction, scanning electron microscopy (SEM) and transmission electron microscopy (TEM) were used.

Robertson, Ian M.↗
NASA NTRS1995

The effect of gravity on the combustion synthesis of Ni-Al and Ni3Al-TiB2 composites from elements

Previous studies on the combustion synthesis of advanced materials indicate that combustion and structure formation mechanisms involve several stages including melting of reactants and products, spreading of the melt, droplet coalescence, diffusion and convection, buoyancy of solid particles, and densification of the liquid product. Most of these processes are affected by gravity. Conducting the combustion synthesis under microgravity conditions is expected to help elucidate the reaction mechanisms. Two systems were examined. The first involves Ni/AI cladded particles, which is an ideal system to examine the individual particle and liquid flow before combustion occurs. For comparison, elemental Ni and Al powders with the same stoichiometry as that of the cladded particles were also used in some experiments. The second system was the Ni3AITiB2 composite in which the Ni3AI (-delta H(sub f) = 153.1 kJ/mol) phase melts during reaction enabling us to examine settling of the liquid phase. The amount of liquid phase was controlled by varying the TiB2 (-delta H(sub f) = 323.8 kJ/mol) content which generates the additional heat. The overall reactions for the two systems can be expressed as follows. System 1: 4Ni + 2AI yields Ni3AI + NiA and System 2: 3Ni + Al + x (Ti + 2B) yields Ni3Al + x(TiB2). For the first system, pellets were pressed directly from the cladded particles, at green densities about 77 +/- 3% of theoretical value. For the second, the pellets were prepared by mixing the elemental reactant powders in the required stoichiometry by ball-milling and then pressing uniaxially at green densities about 70 +/- 3 percent of theoretical. The pellets were cylindrical in shape, 10 mm in diameter and length typically 20-30 mm. The pellet samples were reacted in UHP Argon (1 atm) using the experimental setup and procedure described previously. After reaction, the samples were sectioned axially in order to conduct the microstructural analysis in the longitudinal direction. The phase composition of the reacted product was determined by X-ray diffraction (XRD) and the microstructure was analyzed using scanning electron microscopy (SEM) along with energy dispersive X-ray spectrometry (EDX).

Varma, Arvind↗
NASA NTRS1995

A record of all marker bands found in the upper rivet rows of 2 adjacent bays from a fuselage lap splice joint

A full scale fuselage test article was subjected to 60,000 load cycles (pressurizations) to study the effect of widespread fatigue damage in fuselage structures. Every 10,000 cycles coded marker block loading sequences were used to mark the fracture surfaces of the fatigue cracks propagating within the panel. The loading sequences consisted of series of underloads combined with a series of full pressurizations. The combination of loads and underloads marked the fracture surfaces with marker bands that could later be used to reconstruct the fatigue crack growth history of selected regions within the test article. Thirty rivet holes comprising the upper rivet rows from two adjacent bays (bays #3 and #4) from a fuselage lap splice joint were examined for the purpose of this study. Optical and scanning electron microscopy (SEM) were used to locate the marker bands.

Willard, Scott A.↗
NASA NTRS1996

Solutocapillary Convection Effects on Polymeric Membrane Morphology

Macro voids are undesirable large pores in membranes used for purification. They form when membranes are cast as thin films on a smooth surface by evaporating solvent (acetone) from a polymer solution. There are two un-tested hypotheses explaining the growth of macro voids. One states that diffusion of the non-solvent (water) is solely responsible, while the other states that solutocapillary convection is the primary cause of macro void growth. Solutocapillary convection is flow-caused by a concentration induced surface-tension gradient. Macrovoid growth in the former hypothesis is gravity independent, while in the latter it is opposed by gravity. To distinguish between these two hypotheses, experiments were designed to cast membranes in zero-gravity. A semi-automated apparatus was designed and built for casting membranes during the 20 secs of zero-g time available in parabolic aircraft flight such as NASA's KC-135. The phase changes were monitored optically, and membrane morphology was evaluated by scanning electron microscopy (SEM). These studies appear to be the first quantitative studies of membrane casting in micro-gravity which incorporate real-time data acquisition. Morphological studies of membranes cast at 0, 1, and 1.8 g revealed the presence of numerous, sparse and no macrovoids respectively. These results are consistent with the predictions of the solutocapillary hypothesis of macrovoid growth.

Krantz, William B.↗