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At least 973 records · Page 54

Analysis of Niobium Electropolishing Using a Generalized Distribution of Relaxation Times Method

Using electrochemical impedance spectroscopy, we have devised a method of sensing the microscopic surface conditions on the surface of niobium as it is undergoing an electrochemical polishing (EP) treatment. The method uses electrochemical impedance spectroscopy (EIS) to gather information on the surface state of the electrode without disrupting the polishing reaction. The EIS data is analyzed using a so-called distribution of relaxation times (DRT) method. Using DRT, the EIS data can be deconvolved into discrete relaxation time peaks without any a priori knowledge of the electrode dynamics. By analyzing the relaxation time peaks, we are able to distinguish two distinct modes of the EP reaction. As the polishing voltage is increased, the electrode transitions from the low voltage EP mode, characterized by a single relaxation time peaks, to the high voltage EP mode, characterized by two relaxation time peaks. We theorize that this second peak is caused by the formation of an oxide layer on the electrode. We also find that this oxide induced peak transitions from to a negative relaxation time, which is indicative of a blocking electrode process. By analyzing EPed samples, we show that samples polished in the low voltage mode have significantly higher surface roughness due to grain etching and faceting. We find that the surface roughness of the samples only improves when the oxide film peak is present and in the negative relaxation time region. This shows that EIS combined with DRT analysis can be used to predict etching on EPed Nb. This method can also be performed before or during the EP, which could allow for adjustment of polishing parameters to guarantee a smooth cavity surface finish.

43 PARTICLE ACCELERATORS↗

X-Ray Micro-Computed Tomography of Apollo Samples as a Curation Technique Enabling Better Research

X-ray micro-computed tomography (micro-CT) is a technique that has been used to research meteorites for some time and many others], and recently it is becoming a more common tool for the curation of meteorites and Apollo samples. Micro-CT is ideally suited to the characterization of astromaterials in the curation process as it can provide textural and compositional information at a small spatial resolution rapidly, nondestructively, and without compromising the cleanliness of the samples (e.g., samples can be scanned sealed in Teflon bags). This data can then inform scientists and curators when making and processing future sample requests for meteorites and Apollo samples. Here we present some preliminary results on micro-CT scans of four Apollo regolith breccias. Methods: Portions of four Apollo samples were used in this study: 14321, 15205, 15405, and 60639. All samples were 8-10 cm in their longest dimension and approximately equant. These samples were micro-CT scanned on the Nikon HMXST 225 System at the Natural History Museum in London. Scans were made at 205-220 kV, 135-160 microamps beam current, with an effective voxel size of 21-44 microns. Results: Initial examination of the data identify a variety of mineral clasts (including sub-voxel FeNi metal grains) and lithic clasts within the regolith breccias. Textural information within some of the lithic clasts was also discernable. Of particular interest was a large basalt clast (approx.1.3 cc) found within sample 60639, which appears to have a sub-ophitic texture. Additionally, internal void space, e.g., fractures and voids, is readily identifiable. Discussion: It is clear from the preliminary data that micro-CT analyses are able to identify important "new" clasts within the Apollo breccias, and better characterize previously described clasts or igneous samples. For example, the 60639 basalt clast was previously believed to be quite small based on its approx.0.5 sq cm exposure on the surface of the main mass. These scans show the clast to be approx.4.5 g, however (assuming a density of approx.3.5 g/cc). This is large enough for detailed studies including multiple geo-chronometers. This basalt clast is of particular interest as it is the largest Apollo 16 basalt, and it is the only mid-TiO2 basalt in the Apollo sample suite. By identifying the location of interesting clasts or grains within a sample, we will be able to make more informed decisions about where to cut a sample in order to best expose clasts of interest for future study. Moreover, knowing the location of internal defects (e.g., fractures) will allow more precise chipping and extraction of clasts or grains. By combining micro-CT scans with compositional techniques like micro x-ray fluorescence (particularly on sawn slabs), we will be able to provide even more comprehensive information to scientists trying to best select samples that fit their scientific needs.

Ziegler, R. A.↗

Apollo-11 lunar sample information catalogue

The Apollo 11 mission is reviewed with emphasis on the collection of lunar samples, their geologic setting, early processing, and preliminary examination. The experience gained during five subsequent missions was applied to obtain physical-chemical data for each sample using photographic and binocular microscope techniques. Topics discussed include: binocular examination procedure; breccia clast dexrriptuons, thin section examinations procedure typical breccia in thin section, typical basalt in thin section, sample histories, and chemical and age data. An index to photographs is included.

Kramer, F. E.↗

A Web-Based System for Monitoring and Controlling Multidisciplinary Design Projects

In today's competitive environment, both industry and government agencies are under enormous pressure to reduce the time and cost of multidisciplinary design projects. A number of frameworks have been introduced to assist in this process by facilitating the integration of and communication among diverse disciplinary codes. An examination of current frameworks reveals weaknesses in various areas such as sequencing, displaying, monitoring, and controlling the design process. The objective of this research is to explore how Web technology, in conjunction with an existing framework, can improve these areas of weakness. This paper describes a system that executes a sequence of programs, monitors and controls the design process through a Web-based interface, and visualizes intermediate and final results through the use of Java(Tm) applets. A small sample problem, which includes nine processes with two analysis programs that are coupled to an optimizer, is used to demonstrate the feasibility of this approach.

Salas, Andrea O.↗

Using X-Ray Computed Tomography as a Tool for Preliminary Examination Tool of Current and Future Extraterrestrial Sample Return Missions

The Astromaterials Acquisition and Curation Office at the Johnson Space Center is the past, present, and future home of all of NASA’s astromaterials sample collections. The primary goals of the curation office are to maintain the long-term integrity of the samples and ensure that the samples are distributed for scientific study in a fair, timely, and responsible manner, thus maximizing the return on each sample. Part of the curation process is planning for the future. To this end, we perform fundamental research in advanced curation initiatives to better prepared for future sample return missions. Advanced Curation is tasked with developing procedures, technology, and data sets necessary for curating new sample collections, or getting new results from existing sample collections. As part of these advanced curation efforts, we have installed and are operating a Nikon XTH 320 X-ray Computed Tomography(XCT) system in the JSC curation office with four interchangeable X-ray sources, a large-area detector, and a heavy-duty stage. These instrument characteristics allow us exceptional flexibility to analyze a wide range of sample sizes, from sub-mm soil particles to rocks >10 cm in diameter. The penetrative nature of the XCT scans allows for astromaterials samples to be analyzed within sealed low-density containers (e.g., Teflon bags), preserving the pristinity of the samples. We have begun scanning of the Apollo and Antarctic Meteorite sample suites in order to non-destructively map out lithic clasts (and other features) within the samples. The data from these scans will be made available to scientists via the JSC curation website and the Astromaterials Curation Newsletter. We anticipate sample requests from these “new” lithic clasts identified in these “old” samples. We also anticipate that XCT analyses like these would be useful for future sample return missions, like the OSIRIS REx mission, as well as future sample return missions.

Zeigler, Ryan↗

The Art of Automation: Translating Electron Microscopy Workflows Into Automated Processes

Acquiring data using a scanning transmission electron microscope (STEM) is a complex, multi-step process. The intricacy of the process depends on the type of sample, composition of the material, desired results of the experiment, resolution requirement and other experimental factors. Each experiment presents unique complications, such as sample drift and contamination, that the microscopist must consider when acquiring data. All these challenges are handled fluidly and expertly by experienced microscopists, but to reach new levels of innovation in material development, including greater reproducibility, throughput, and precision, the automation of these workflows is essential. The initial phase of this work involved translating intuition-based workflows into discrete, programmable steps. Some common key stages in STEM workflows are the initial tuning, scanning the sample for areas of interest, and then acquiring the data. Each stage can be broken further into specific parameter adjustments, such as aberration correction and dwell time optimization, depending on the experiment. When deconstructing various experiments each step was assessed for automation feasibility based on the amount of real time operator decisions. There are steps that lend themselves to automation more readily than others, such as course focusing and sample screening, but there is potential for full automation of all stages with time. As an initial step, an automated montage routine was developed, allowing for the efficient acquisition of large portions of the sample without requiring continuous intervention from the operator. The automation of this small process of the procedure demonstrates the value of this capability. A major challenge in automation arises from discrepancies between commanded, reported and actual stage movements. Using systematic tests, stage movement was quantified. This error can be corrected algorithmically for more accurate workflows in the future. Expanding automation capabilities would result in larger, more efficient data acquisition which allows for more robust statistical analysis. Additionally, this work lays the groundwork for a closed loop system where machine learning algorithms would intake automatically acquired data and make real time decisions. By progressively automating this instrument, this work establishes the foundation for fully automated experimentation in transmission electron microscopy.

97 MATHEMATICS AND COMPUTING↗

Spectrum of carbonaceous-chondrite fission xenon

Estimations of the fission spectrum in xenon isotopes from the progenitor of the strange carbonaceous-chondrite xenon must take account of p-process nucleosynthesis if the latter is the source of anomalous Xe-124, 126. Sample calculations of the p-process yields illustrate the magnitude of the effect, which can greatly increase the estimated Xe-132 fission yield.

Clayton, D. D.↗

The asymmetric distribution of satellite galaxy velocities

Companion galaxies tend to have redshifts that exceed that of their associated primary. We show that the latest sample of satellite galaxies (from Zaritsky et al.) corroborates this assertion. We examine whether selection biases and contamination by galaxies that are not physical satellites can create the observed velocity asymmetry. As shown by Valtonen and Byrd (1986) for previous samples, simple models of the selection process reproduce the sense of the asymmetry, but not its magnitude unless the samples are dominated by interlopers. We expand on this model by using numerical simulations that include a simple model of galaxy clustering, and demonstrate that clustering can increase the magnitude of the expected asymmetry for a particular level of contamination. Depending on input assumptions, these models imply 1 sigma lower limits on the contamination level in the Zaritsky et al. (1992) sample of between 8 and 20 percent. Using the results from the analysis of that sample and the models, we conclude that, for the type of satellite galaxy sample discussed, here, a moderate level of contamination (about 10 percent) is sufficient to account for the observed asymmetry.

Zaritsky, Dennis↗

Method and Apparatus for High Data Rate Demodulation

A method to demodulate BPSK or QPSK data using clock rates for the receiver demodulator of one-fourth the data rate is presented. This is accomplished through multirate digital signal processing techniques. The data is sampled with an analog-to-digital converter and then converted from a serial data stream to a parallel data stream. This signal processing requires a clock cycle four times the data rate. Once converted into a parallel data stream, the demodulation operations including complex baseband mixing, lowpass filtering, detection filtering, symbol-timing recovery, and carrier recovery are all accomplished at a rate one-fourth the data rate. The clock cycle required is one-sixteenth that required by a traditional serial receiver based on straight convolution. The high rate data demodulator will demodulate BPSK, QPSK, UQPSK, and DQPSK with data rates ranging from 10 Mega-symbols to more than 300 Mega-symbols per second. This method requires less clock cycles per symbol tan traditional serial convolution techniques.

Gerald J Grebowsky↗

Measurements of the sampling volume of an infrared laser doppler velocimeter for the study of feasibility of simultaneous three-dimensional velocity profile mapping

High resolution incoherent mapping of the sampling volume was performed to determine the three dimensional profile of the volume of the beam from which information can be obtained by scattering. The incoherent sampling volume of the infrared laser Doppler velocimeter was found to be heavily dependent upon the configuration of the outgoing laser beam. In general when only half the beam is allowed to focus at the focal plane, the x, y traverses indicate a broader beam with nominal side lobes. However, if the total beam is permitted to impinge on the focal plane there is substantial narrowing of the beam with increased maximum intensity and an increase in side lobes. The double maximum indicated by the coherent sampling volume appears to be an artifact of the scanning process not a fundamental entity of the sampling volume.

Bond, R. L.↗

Generalized multi-dimensional sampling theory and applications in optical systems.

Summary of the generalized sampling theory developed by Peterson (1963) and others, which treated multidimensional impulse-modulation periodic sampling, applicable to any multidimensional process. Particular attention is given to the two-dimensional case (N = 2) for which applications in optical systems are proposed. The efficiency of sampling geometries, and digital holography and sampling theory are considered.

Hopper, W. A.↗

Macrosegregation in undercooled Pb-Sn eutectic alloys

A novel technique resulting in large undercoolings in bulk samples (23g) of lead-tin eutectic alloy is described. Samples of eutectic composition were processed with undercoolings ranging from 4 to 20 K and with cooling rates varying between 0.04 to 4 K/sec. The final macrostructure of undercooled samples depends on both the initial undercooling of the melt and the cooling rate. Gravity-driven segregation is found to increase with increasing undercooling. A eutectic Pb-Sn alloy undercooled at 20 K and cooled at 4 K/sec had a composition of about Pb-72 wt pct Sn at the top and 55 pct Sn at the bottom. Macrosegregation in these undercooled lead-tin eutectic alloys is shown to be primarily due to a sink/float mechanism caused by the difference in density of the solid and liquid phases and the undercooling and nucleation behavior of the alloy.

De Groh, H. C., III↗

Containerless processing of undercooled melts

All practical solidification processes involve some level of melt undercooling. Usually in bulk liquids crystallization is initiated at a heterogeneous nucleation site at low undercooling. The realization of appreciable levels of liquid undercooling requires some control over the kinetics of crystal nucleation. One level of control is available in containerless processing where the capability to melt and solidify samples without a container removes a major source of impurities and heterogeneous nucleation sites which can be effective in promoting large undercooling and in studying other potential nucleants. The microgravity environment offers a unique opportunity for containerless processing of large liquid samples with negligible melt disturbance and continuous temperature measurement throughout processing. Perhaps the most important potential for microgravity containerless processing lies in the significant structural control to develop distinct microstructures and metastable phases during solidification at high undercooling.

Perepezko, J. H.↗

A method for determining the weak statistical stationarity of a random process

A method for determining the weak statistical stationarity of a random process is presented. The core of this testing procedure consists of generating an equivalent ensemble which approximates a true ensemble. Formation of an equivalent ensemble is accomplished through segmenting a sufficiently long time history of a random process into equal, finite, and statistically independent sample records. The weak statistical stationarity is ascertained based on the time invariance of the equivalent-ensemble averages. Comparison of these averages with their corresponding time averages over a single sample record leads to a heuristic estimate of the ergodicity of a random process. Specific variance tests are introduced for evaluating the statistical independence of the sample records, the time invariance of the equivalent-ensemble autocorrelations, and the ergodicity. Examination and substantiation of these procedures were conducted utilizing turbulent velocity signals.

Sadeh, W. Z.↗

The SASS scattering coefficient algorithm

This paper describes the algorithms used to convert engineering unit data obtained from the Seasat-A satellite scatterometer (SASS) to radar scattering coefficients and associated supporting parameters. A description is given of the instrument receiver and related processing used by the scatterometer to measure signal power backscattered from the earth's surface. The applicable radar equation used for determining scattering coefficient is derived. Sample results of SASS data processed through current algorithm development facility (ADF) scattering coefficient algorithms are presented which include scattering coefficient values for both water and land surfaces. Scattering coefficient signatures for these two surface types are seen to have distinctly different characteristics. Scattering coefficient measurements of the Amazon rain forest indicate the usefulness of this type of data as a stable calibration reference target.

Bracalente, E. M.↗

Production of superconductor/carbon bicomponent fibers

Certain materials are unable to be drawn or spun into fiber form due to their improper melting characteristics or brittleness. However, fibrous samples of such materials are often necessary for the fabrication of intricate shapes and composites. In response to this problem, a unique process, referred to as the piggyback process, was developed to prepare fibrous samples of a variety of nonspinnable ceramics. In this technique, specially produced C-shaped carbon fibers serve as micromolds to hold the desired materials prior to sintering. Depending on the sintering atmosphere used, bicomponent or single component fibers result. While much has been demonstrated worldwide concerning the YBa2Cu3O(7-x) superconductor, fabrication into unique forms has proven quite difficult. However, a variety of intricate shapes are necessary for rapid commercialization of the superconducting materials. The potential for producing fibrous samples of the YBa2Cu3O(7-x) compound by the piggyback process is being investigated. Various organic and acrylic materials were investigated to determine suspending ability, reactivity with the YBa2Cu3O(7-x) compound during long term storage, and burn out characteristics. While many questions were answered with respect to the interfacial reactions between YBa2Cu3O(7-x) and carbon, much work is still necessary to improve the quality of the sintered material if the fibers produced are to be incorporated into useful composites or cables. Additional research is necessary to evaluate quality of the barrier layer during long soakings at the peak temperature; adjust the firing schedule to avoid microcracking and improve densification; and increase the solids loading in the superconductive suspension to decrease porosity.

Wise, S. A.↗

Production of superconductor/carbon bicomponent fibers

Certain materials are unable to be drawn or spun into fiber form due to their improper melting characteristics or brittleness. However, fibrous samples of such materials are often necessary for the fabrication of intricate shapes and composites. In response to this problem, a unique process, referred to as the piggyback process, was developed to prepare fibrous samples of a variety of nonspinnable ceramics. In this technique, specially produced C shaped carbon fibers serve as micromolds to hold the desired materials prior to sintering. Depending on the sintering atmosphere used, bicomponent or single component fibers result. While much has been shown worldwide concerning the YBa2Cu3O(7-x) superconductor, fabrication into unique forms has proven quite difficult. However, a variety of intricate shapes are necessary for rapid commercialization of the superconducting materials. The potential for producing fibrous samples of the YBa2Cu3O(7-x) compound by the piggyback process is being studied. Various organic and acrylic materials were studied to determine suspending ability, reactivity with the YBa2Cu3O(7-x) compound during long term storage, and burn out characteristics. While many questions were answered with respect to the interfacial reactions between YBa2Cu3O(7-x) and carbon, much work is still necessary to improve the quality of the sintered material if the fibers produced are to be incorporated into useful composite or cables.

Wise, S. A.↗

Rapid monitoring of fermentations: a feasibility study on biological 2,3-butanediol production

2,3-butanediol (2,3-BDO) is an economically important platform chemical that can be produced by the fermentation of sugars using an engineered strain of Zymomonas mobilis . These fermentations require continuous monitoring and modification of fermentation conditions to maximize 2,3-BDO yields and minimize the production of the undesired coproducts glycerol and acetoin. Because of the time required for sampling and off-line chromatographic measurement of fermentation samples, the ability of fermentation scientists to modify fermentation conditions in a timely manner is limited. The goal of this study was to test if near-infrared spectroscopy (NIRS) along with multivariate statistics could reduce the time needed for this analysis and enable real-time monitoring and control of the fermentation. In this work we developed partial least squares (PLS) calibration models to predict the concentrations of glucose, xylose, 2,3-BDO, acetoin, and glycerol in fermentations via NIRS using two different spectrometers and two different spectroscopy modalities. We first evaluated the feasibility of rapid NIRS monitoring through experiments where we measured the signals from each analyte of interest and built NIRS-based PLS models using spectra from synthetic samples containing uncorrelated concentrations of these analytes. All analytes showed unique spectral signatures, and this initial modeling showed that all analytes could be detected simultaneously. We then began work with samples from laboratory fermentation experiments and tested the feasibility of regression model development across two spectral collection modalities (at-line and on-line) and two instruments: a laboratory-grade instrument and a low-cost instrument with a more limited spectral range. All modalities showed promise in the ability to monitor Z. mobilis fermentations of glucose and xylose to 2,3-BDO. The low-cost instrument displayed a lower signal-to-noise ratio than the laboratory-grade instrument, which led to comparatively lower performance overall, but still provided sufficient accuracy to monitor fermentation trends. While the ease of use of on-line monitoring systems was favored as compared to at-line systems due to the lack of sampling required and potential for automated process control, we observed some decrease in performance due to the additional complexity of the sample matrix. We have demonstrated that NIRS combined with multivariate analysis can be used for at-line and on-line monitoring of the concentrations of glucose, xylose, 2,3-BDO, acetoin, and glycerol during Z. mobilis fermentations. The decrease in signal-to-noise ratio when using a low-cost spectrometer led to greater prediction error than the laboratory-grade spectrometer for at-line monitoring. The on-line monitoring modality showed great promise for real time process control via NIRS.

09 BIOMASS FUELS↗