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At least 505 records · Page 28

Characterization of Surface Features in Detached Grown GeSi Crystals

The growth of detached crystals by the Bridgman technique, in which the growing crystal is not in contact with the crucible wall, has been observed both on earth and in microgravity conditions. At present, the mechanisms contributing to the detachment are not completely understood and until recently detachment has not been reproducibly obtained. It is commonly understood that the main factors that promote the occurrence of detached growth include: high contact angle between the melt and the crucible material, high growth angle, and a pressure difference between the annular gap around the solid below the melt and the volume above the melt along the meniscus. These parameters were varied in Bridgman growth experiments to determine the conditions required to achieve detached growth terrestrially in Ge and GeSi alloys. These experiments are in preparation for experiments on the International Space Station (ISS). The detailed objectives of the flight experiments and a description of the growth methods employed are the subject of another presentation at this Congress. Detached crystals were achieved repeatedly in pyrolytic boron nitride ampoules when a pressure difference was employed. All crystals, except for those grown in fused silica ampoules, were easily removed from their containers; however, this fact alone is not sufficient to infer detached growth. Detachment was verified by comparing profilometer measurements of the radius of the samples with observations of the sample surfaces using optical and electron microscopy. The surfaces of the attached areas of the crystals had the same shape and surface texture as the interior crucible wall. Regions of detached growth contained many unique features and crystal facets could usually be observed. Several of these surface features have been correlated with mechanisms of detachment or free surface growth in general and others to processing events or conditions. These results will be compared with observations of surface features on detached regions of microgravity grown crystals.

Cobb, S. D.↗

Bridgman Growth of Detached GeSi Crystals

The growth of detached crystals by the Bridgman technique, in which the growing crystal is not in contact with the crucible wall, has been observed both on earth and in microgravity conditions. Such detachment has particularly been in evidence in microgravity experiments, where the pressure head of the molten sample is absent. At present, the mechanisms contributing to the detachment are not completely understood and until recently detachment has not been reproducibly obtained. Key parameters which must be considered are the contact angle between the melt and the crucible and the growth angle. Another essential parameter is the pressure difference between the annular gap around the solid below the melt and the volume above the melt. Here we present results of the growth of Ge(0.98)Si(0.02) using adjustments in the applied temperature profile to control the pressure difference between the bottom and top of the melt. The technique is less susceptible to sample contamination than controlling the pressure by connecting the crucible to external gas sources. Using this technique, a pressure difference is created by decreasing the temperature in the volume above the melt while the sample is molten but prior to growth. A maximum pressure difference approximately equal to the pressure head of the molten sample can thus be obtained. Several GeSi crystals were grown in pyrolitic boron nitride crucibles. When a pressure difference was applied, samples were reproducibly grown mostly detached. For comparison, samples were also grown in a configuration in which gas could pass freely between the gap below the melt and the volume above the melt and no pressure difference could be established. These samples were initially attached. Existence of detachment was determined both by measuring the radius of the samples with a profilometer and by observations of the sample surfaces with optical and electron microscopy. The gap thickness between the crucible and detached crystal was on the order of 10 micron. The surfaces of the attached areas of the crystals had the same shape as the interior crucible wall whereas in the detached areas the crystal facets could usually be observed.

Volz, M. P.↗

Defect Density Comparison of Detached versus Attached Bridgman Grown Germanium Crystals

Semiconductor Bridgman growth without contact between the growing crystal and the growth ampoule has been observed on Earth in the last few years during several experiments. Previously, this so-called detached or dewetted growth phenomenon occurred preferentially under microgravity conditions due to the absence of the hydrostatic pressure. Many theoretical as well as experimental investigations helped to provide a better understanding of the mechanism and to identify the parameters leading to the detachment. Thus, recent attempts to get stable detached growth under terrestrial conditions by Duffar et al. growing III-V compounds and our own group with germanium and germanium-silicon alloys were frequently successful. At this conference we present the results of several germanium growth experiments performed in pyrolytic boron nitride containers. To exert an influence on the pressure ratio above and below the melt we used closed-bottom and open-bottom containers. This resulted in mainly detached-grown single crystals with the closed-bottom crucibles and attached single crystals with the open-bottom tubes. Evidence of detached growth is obtained from the crystal surface with a combination of axial profilometer scans and optical and electron microscopy. Detailed investigations of the defect structure, which is the main focus of this presentation, have shown an improvement of the crystal quality in the detached-grown samples, with a strong reduction of the etch pit density by about two orders of magnitude.

Schweizer, M.↗

Bridgman Growth of Detached GeSi Crystals

Ge(1-x)Si(x)(0 less than x less than 0.12) has been grown by the vertical Bridgman technique using adjustments in the applied temperature profile to control the pressure difference between the bottom and top of the melt. Using this technique, a pressure difference is created by decreasing the temperature in the gas volume above the melt while the sample is molten but prior to growth. A maximum pressure difference approximately equal to the hydrostatic pressure of the molten sample can thus be obtained. Several GeSi crystals were grown in pyrolitic boron nitride ampoules. When a pressure difference was applied, samples were reproducibly grown mostly detached. For comparison, samples were also grown in a configuration in which gas could flow freely between the gap below the melt and the volume above the melt and no pressure difference could be established. These samples were initially attached. Existence of detachment was determined both by measuring the surface roughness of the samples with a profilometer and by observations of the sample surfaces with optical and electron microscopy.

Volz, M. P.↗

Detached Bridgman Growth of Germanium and Germanium-Silicon Alloy Crystals

Earth based experiments on the science of detached crystal growth are being conducted on germanium and germanium-silicon alloys (2 at% Si average composition) in preparation for a series of experiments aboard the International Space Station (ISS). The purpose of the microgravity experiments includes differentiating among proposed mechanisms contributing to detachment, and confirming or refining our understanding of the detachment mechanism. Because large contact angle are critical to detachment, sessile drop measurements were used to determine the contact angles as a function of temperature and composition for a large number of substrates made of potential ampoule materials. Growth experiments have used pyrolytic boron nitride (pBN) and fused silica ampoules with the majority of the detached results occurring predictably in the pBN. The contact angles were 173 deg (Ge) and 165 deg (GeSi) for pBN. For fused silica, the contact angle decreases from 150 deg to an equilibrium value of 117 deg (Ge) or from 129 deg to an equilibrium value of 100 deg (GeSi) over the duration of the experiment. The nature and extent of detachment is determined by using profilometry in conjunction with optical and electron microscopy. The stability of detachment has been analyzed, and an empirical model for the conditions necessary to achieve sufficient stability to maintain detached growth for extended periods has been developed. Results in this presentation will show that we have established the effects on detachment of ampoule material, pressure difference above and below the melt, and silicon concentration; samples that are nearly completely detached can be grown repeatedly in pBN.

Szofran, F. R.↗

Characterization of Surface Features in Detached Grown GeSi Crystals

The growth of detached crystals by the Bridgman technique, in which the growing crystal is not in contact with the crucible wall, has been observed both on earth and in microgravity conditions. At present, the mechanisms contributing to the detachment are not completely understood and until recently detachment has not been reproducibly obtained. It is commonly understood that the main factors that promote the occurrence of detached growth include: high contact angle between the melt and the crucible material, high growth angle, and a pressure difference between the annular gap around the solid below the melt and the volume above the melt along the meniscus. These parameters were varied in Bridgman growth experiments to determine the conditions required to achieve detached growth terrestrially in Ge and GeSi alloys. These experiments are in preparation for experiments on the International Space Station (ISS). The detailed objectives of the flight experiments and a description of the growth methods employed are the subject of another presentation at this Conference. Detached crystals were achieved repeatedly in pyrolytic boron nitride ampoules when a pressure difference was employed. All crystals, except for those grown in fused silica ampoules, were easily removed from their containers, however, this fact alone is not sufficient to infer detached growth. Detachment was verified by comparing profilometer measurements of the radius of the samples with observations of the sample surfaces using optical and electron microscopy. The surfaces of the attached areas of the crystals had the same shape and surface texture as the interior crucible wall. Regions of detached growth contained many unique features and crystal facets could usually be observed. Several of these surface features have been correlated with mechanisms of detachment or free-surface growth and others to processing events or conditions.

Cobb, S. D.↗

Bridgman Growth of Detached GeSi Crystals

Ge(1-x)Si(x) (0 less than x less than 0.12) has been grown by the vertical Bridgman technique using adjustments in the applied temperature profile to control the pressure difference between the bottom and top of the melt. Using this technique. a pressure difference is created by decreasing the temperature in the gas volume above the melt while the sample is molten but prior to growth. A maximum pressure difference approximately equal to the hydrostatic pressure of the molten sample can thus be obtained. Several GeSi crystals were grown in pyrolitic boron nitride ampoules. When a pressure difference was applied, samples were reproducibly grown mostly detached. For comparison, samples were also grown in a configuration in which gas could flow freely between the gap below the melt and the volume above the melt and no pressure difference could be established. These samples were initially attached. Existence of detachment was determined both by measuring the surface roughness of the samples with a profilometer and by observations of the sample surfaces with optical and electron microscopy.

Volz, M. P.↗

Characterization of Two Microbial Isolates from Andean Lakes in Bolivia

We are currently investigating the biological population present in the highest and least explored perennial lakes on earth in the Bolivian and Chilean Andes, including several volcanic crater lakes of more than 6000 m elevation, in combination of microbiological and molecular biological methods. Our samples were collected in saline lakes of the Laguna Blanca Laguna Verde area in the Bolivian Altiplano and in the Licancabur volcano crater (27 deg. 47 min S/67 deg. 47 min. W) in the ongoing project studying high altitude lakes. The main goal of the project is to look for analogies with Martian paleolakes. These Bolivian lakes can be described as Andean lakes following the classification of Chong. We have attempted to isolate pure cultures and phylogenetically characterize prokaryotes that grew under laboratory conditions. Sediment samples taken from the Licancabur crater lake (LC), Laguna Verde (LV), and Laguna Blanca (LB) were analyzed and cultured using enriched liquid media under both aerobic and anaerobic conditions. All cultures were incubated at room temperature (15 to 20 C) and under light exposure. For the reported isolates, 36 hours incubation were necessary for reaching optimal optical densities to consider them viable cultures. Ten serial dilutions starting from 1% inoculum were required to obtain a suitable enriched cell culture to transfer into solid media. Cultures on solid medium were necessary to verify the formation of colonies in order to isolate pure cultures. Different solid media were prepared using several combinations of both trace minerals and carbohydrates sources in order to fit their nutrient requirements. The microorganisms formed individual colonies on solid media enriched with tryptone, yeast extract and sodium chloride. Cells morphology was studied by optical and electronic microscopy. Rodshape morphologies were observed in most cases. Total bacterial genomic DNA was isolated from 50 ml late-exponential phase culture by using the CTAB miniprep protocol. The 16S rRNA genes were amplified by PCR using both Bacteria- and Archaeauniversal primer sets: 27f and 1492r, 21f and 1492r respectively. Sequences of 16S rRNA gene were determined and initially compared with reference sequences contained in the EMBL nucleotide sequence database by using the BLAST program and were subsequently aligned with 16S rRNA reference sequences in the ARB package (http://www.mikro.biologie.tu-muenchen.de). Aligned sequences were inserted within a stable phylogenetic tree by using the ARB parsimony tool. In this work we report the morphology and phylogenetic characterization of two isolates belonged to Laguna Blanca sediments.

Demergasso, C.↗

Reduction of Defects in Germanium-Silicon

Crystals grown without contact with a container have far superior quality to otherwise similar crystals grown in direct contact with a container. In addition to float-zone processing, detached- Bridgman growth is a promising tool to improve crystal quality, without the limitations of float zoning or the defects introduced by normal Bridgman growth. Goals of this project include the development of the detached Bridgman process to be reproducible and well understood and to quantitatively compare the defect and impurity levels in crystals grown by these three methods. Germanium (Ge) and germanium-silicon (Ge-Si) alloys are being used. At MSFC, we are responsible for the detached Bridgman experiments intended to differentiate among proposed mechanisms of detachment, and to confirm or refine our understanding of detachment. Because the contact angle is critical to determining the conditions for detachment, the sessile drop method was used to measure the contact angles as a function of temperature and composition for a large number of substrates made of potential ampoule materials. Growth experiments have used pyrolytic boron nitride (pBN) and fused silica ampoules with the majority of the detached results occurring predictably in the pBN. Etch pit density (EPD) measurements of normal and detached Bridgman-grown Ge samples show a two order of magnitude improvement in the detached-grown samples. The nature and extent of detachment is determined by using profilometry in conjunction with optical and electron microscopy. The stability of detachment has been analyzed, and an empirical model for the conditions necessary to achieve sufficient stability to maintain detached growth for extended periods has been developed. We have investigated the effects on detachment of ampoule material, pressure difference above and below the melt, and Si concentration; samples that are nearly completely detached can be grown repeatedly in pBN. Current work is concentrated on developing a method to make in situ pressure measurements in the growth ampoules.

Source record↗

Tribometer for Lubrication Studies in Vacuum

The NASA Lewis Research Center has developed a new way to evaluate the liquid lubricants used in ball bearings in space mechanisms. For this evaluation, a liquid lubricant is exercised in the rolling contact vacuum tribometer shown in the photo. This tribometer, which is essentially a thrust bearing with three balls and flat races, has contact stresses similar to those in a typical preloaded, angular contact ball bearing. The rotating top plate drives the balls in an outward-winding spiral orbit instead of a circular path. Upon contact with the "guide plate," the balls are forced back to their initial smaller orbit radius; they then repeat this spiral orbit thousands of times. The orbit rate of the balls is low enough, 2 to 5 rpm, to allow the system to operate in the boundary lubrication regime that is most stressful to the liquid lubricant. This system can determine the friction coefficient, lubricant lifetime, and species evolved from the liquid lubricant by tribodegradation. The lifetime of the lubricant charge is only few micrograms, which is "used up" by degradation during rolling. The friction increases when the lubricant is exhausted. The species evolved by the degrading lubricant are determined by a quadrupole residual gas analyzer that directly views the rotating elements. The flat races (plates) and 0.5-in.-diameter balls are of a configuration and size that permit easy post-test examination by optical and electron microscopy and the full suite of modern surface and thin-film chemical analytical techniques, including infrared and Raman microspectroscopy and x-ray photoelectron spectroscopy. In addition, the simple sphere-on-a-flat-plate geometry allows an easy analysis of the contact stresses at all parts of the ball orbit and an understanding of the frictional energy losses to the lubricant. The analysis showed that when the ball contacts the guide plate, gross sliding occurs between the ball and rotating upper plate as the ball forced back to a smaller orbit radius. The friction force due to gross sliding is sensed by the piezoelectric force transducer behind the guide plate and furnishes the coefficient of friction for the system. This tribometer has been used to determine the relative lifetimes of Fomblin Z-25, a lubricant often used in space mechanisms, as a function of the material of the plates against which it was run. The balls were 440C steel in all cases; the plate materials were aluminum, chromium (Cr), 440C steel (17 wt % Cr), and 4150 steel (1 wt % Cr). As shown in the bar graph, the lifetime is greatest for the plate material with least chromium, thus implicating chromium as a tribochemically active element attacking Fomblin Z-25.

Pepper, Stephen V.↗

Analysis of Black Bearing Balls from a Space Shuttle Body Flap Actuator

A significantly deteriorated ball bearing mechanism from a body flap actuator on Space Shuttle OV-103 was disassembled and the balls submitted for analysis in conjunction with Return to Flight activities. The OV-103 balls, referred to as the "black balls", were subjected to X-ray photoelectron spectroscopy (XPS), Fourier transform infrared (FT-IR) and Raman micro spectroscopy, surface profilometry, and optical and electron microscopy. The spectroscopic results in combination with microscopy analysis allowed a determination of the lubricant degradation pathway. The chemical attack mechanism does not adequately explain the unique visual appearance of the black balls. Numerous efforts have unsuccessfully focused on duplication of the phenomena causing this unique surface structure and appearance of the black balls. Further detail will be presented supporting these conclusions along with plausible explanations of the unique black appearance to the balls.

Sovinski, Marjorie F.↗

Analysis of Cometary Dust Impact Residues in the Aluminum Foil Craters of Stardust

In January 2006, the sample return capsule from NASA s Stardust spacecraft successfully returned to Earth after its seven year mission to comet Wild-2. While the principal capture medium for comet dust was low-density graded silica aerogel, the 1100 series aluminum foil (approximately 100 m thick) which wrapped around the T6064 aluminum frame of the sample tray assembly (STA) contains micro-craters that constitute an additional repository for Wild-2 dust. Previous studies of similar craters on spacecraft surfaces, e.g. the Long Duration Exposure Facility (LDEF), have shown that impactor material can be preserved for elemental and mineralogical characterization, although the quantity of impact residue in Stardust craters far exceeds previous missions. The degree of shock-induced alteration experienced by the Wild-2 particles impacting on foil will generally be greater than for those captured in the low-density aerogel. However, even some of the residues found in LDEF craters showed not only survival of crystalline silicates but even their solar flare tracks, which are extremely fragile structures and anneal at around 600 C. Laboratory hypervelocity experiments, using analogues of Wild-2 particles accelerated into flight-grade foils under conditions close to those of the actual encounter, showed retention of abundant projectile residues at the Stardust encounter velocity of 6.1 km/s. During the preliminary examination (PE) of the returned foils, using optical and electron microscopy studies, a diverse range in size and morphologies of micro-craters was identified. In this abstract we consider the state of residue preservation in a diverse range of craters with respect to their elemental composition and inferred mineralogy of the original projectiles.

Graham, G. A.↗

Degradation of Beta Cloth Covering for a Battery Orbital Replacement Unit in Low Earth Orbit

Samples from the beta cloth cover for a battery orbit replaceable unit from the International Space Station (ISS) were characterized using optical and electron microscopy, UV-vis-NIR spectrophotometry, and x-ray energy dispersive spectroscopy. Results showed that in areas where the fabric was exposed to solar radiation the absorptance increased by as much as 20 percent, and the peak difference was in the ultraviolet, indicating that the increased absorptance may have been due to radiation. The emissivity of the material over a temperature range of 300 to 700 K was essentially unchanged.

Solar Physics↗

Degradation of Beta-Cloth Covering for a Battery Orbital Replacement Unit in Low Earth Orbit

Samples from the B-cloth cover for a battery orbit replaceable unit from the International Space Station were characterized using optical and electron microscopy, UV-vis-NIR spectrophotometry, and x-ray energy dispersive spectroscopy. Results showed that in areas where the fabric was exposed to solar radiation the absorptance increased by as much as 20 percent, and the peak difference was in the ultraviolet, indicating that the increased absorptance may have been due to radiation. The emissivity of the material over a temperature range of 300 - 700 K was essentially unchanged.

Solar Physics↗

Mechanisms of Interfacial Mixing in the Blown Powder Deposition of Inconel 625 to Copper Alloy for Liquid Rocket Engine Applications

There is an increasing need for functional materials to support high heat flux applications and optimize weight by using bimetallic additive manufacturing (AM). While one promising fabrication technology is the use of blown powder directed energy deposition (DED) AM, challenges remain with bi-metallic combinations. Prominent among these challenges is the need to understand mixing of materials at the bimetallic interface for forming stronger, more durable and reliable joints to extend the versatility of AM into critical applications. One application is the manufacturing of combustion chambers with copper-alloy liners and Superalloy structural jackets. In this application, material combinations are selected for effective heat dissipation, using copper, and retention of strength at high temperatures using Inconel 625. Currently, the dominant problem with this configuration is the highly variable strength of the interface and its correlation with deposition parameters. In this study, samples were fabricated at several vendors with Inconel 625 deposited onto wrought C-18150 (Cu-Cr-Zr) to form a bimetallic interface. Characterization of the interfaces were achieved through optical and electron microscopy, mechanical testing of mini tensile specimens, and electron dispersion spectroscopy to understand diffusion and bulk mixing behaviors at the joint. A theoretical framework was constructed in the context of solidification and mixing mechanisms to explain the resulting differences in the interface. This qualitative approach utilized a fluid dynamics perspective to sum the order of magnitudes of the various acting forces on the weld pool during deposition to predict convection trends based off known parameters. The predicted trends for each vendor are compared to obtain a better understanding of how mixing in the molten pool varied based on deposition parameters.

Additive Manufacturing↗

Reliability of area array packages with 1500-2500 I/Os

This report first provides a literature survey for designing, manufacturing, and reliability test results for area array packages with 1500 to 2500 inputs/outputs (I/Os). It then presents test matrix on design, yield, and workmanship defects on assembly and environmental testing, including thermal cycle and mechanical drop-test evaluation results for FCBGA1704, FPBGA432, and PBGA676 I/Os packages assembled onto printed circuit/wiring boards (PCBs/PWBs). Finally, it summarizes lessons learned from test results for assembly and environmental testing along with optical, scanning electron microscopy (SEM), and x-ray photomicrographs showing damage progress.

Ghaffarian, Reza↗

Investigation into Interfacial Mixing Behavior of Blown Powder Deposited Inconel 625-Copper Alloy Bimetallic for Improvement of Bimetallic Joint Strength

Use of laser blown powder, directed energy deposition (DED) provides a method for fabrication of bimetallic functional materials for high heat flux applications. However, this relatively new process currently has a low technology readiness level (TRL). Key to increasing the TRL is a better understanding of the factors that control mixing of the bi-metallic materials at the interface. The resulting interfaces in specimens obtained from three vendors were characterized using optical and electron microscopy with electron dispersion spectroscopy in addition to mechanical testing. Based on the range of process parameters and resulting interfaces, a model is being developed to predict interfacial mixing for development of specifications for improved and repeatable microstructures.

Additive Manufacturing↗

Shock effects on hydrous minerals and implications for carbonaceous meteorites

The effect of shock loading over the pressure range of 29-59 GPa on the shock-recovered specimens of antigorite serpentine, Mg3Si2O5(OH)4, were investigated employing infrared (IR) spectroscopy, thermogravimetric analysis, and optical and scanning electron microscopy. With increasing shock pressure, there was an increase in H2O IR absorption peaks at the expense of OH peaks, while the changes in SiO bond vibration modes were identical to those seen for other, nonhydrous minerals. Thermogravimetric results on vented assembly samples showed linear relationships between the shock pressure and both the length of dehydration interval and the effective activation energy for releasing post-shock structural water. Optical and scanning electron microscopy revealed gas bubbles, which appeared to be injected into zones of partial melting, and vesicular dark veins distributed throughout the shocked samples. It is suggested that shock loading of hydrous minerals would release and redistribute free water in the regoliths of carbonaceous chondrite parent bodies, giving rise to observed hydrous alterations.

Lange, M. A.↗