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At least 73 records · Page 4

Materials Combustion Testing and Combustion Product Sensor Evaluations in FY12

NASA Centers continue to collaborate to characterize the chemical species and smoke particles generated by the combustion of current space-rated non-metallic materials including fluoropolymers. This paper describes the results of tests conducted February through September 2012 to identify optimal chemical markers both for augmenting particle-based fire detection methods and for monitoring the post-fire cleanup phase in human spacecraft. These studies follow up on testing conducted in August 2010 and reported at ICES 2011. The tests were conducted at the NASA White Sands Test Facility in a custom glove box designed for burning fractional gram quantities of materials under varying heating profiles. The 623 L chamber was heavily instrumented to quantify organics (gas chromatography/mass spectrometry), inorganics by water extraction followed by ion chromatography, and select species by various individual commercially-available sensors. Evaluating new technologies for measuring carbon monoxide, hydrogen cyanide, hydrogen fluoride, hydrogen chloride and other species of interest was a key objective of the test. Some of these sensors were located inside the glovebox near the fire source to avoid losses through the sampling lines; the rest were located just outside the glovebox. Instruments for smoke particle characterization included a Tapered Element Oscillating Microbalance Personal Dust Monitor (TEOM PDM) and a TSI Dust Trak DRX to measure particle mass concentration, a TSI PTrak for number concentration and a thermal precipitator for collection of particles for microscopic analysis. Materials studied included Nomex(R), M22759 wire insulation, granulated circuit board, polyvinyl chloride (PVC), Polytetrafluoroethylene (PTFE), Kapton(R), and mixtures of PTFE and Kapton(R). Furnace temperatures ranged from 340 to 640 C, focusing on the smoldering regime. Of particular interest in these tests was confirming burn repeatability and production of acid gases with different fuel mixture compositions, as well as the dependence of aerosol concentrations on temperature.

Combustion↗

Spacecraft Fire Safety Research at NASA Glenn Research Center

Appropriate design of fire detection systems requires knowledge of both the expected fire signature and the background aerosol levels. Terrestrial fire detection systems have been developed based on extensive study of terrestrial fires. Unfortunately there is no corresponding data set for spacecraft fires and consequently the fire detectors in current spacecraft were developed based upon terrestrial designs. In low gravity, buoyant flow is negligible which causes particles to concentrate at the smoke source, increasing their residence time, and increasing the transport time to smoke detectors. Microgravity fires have significantly different structure than those in 1-g which can change the formation history of the smoke particles. Finally the materials used in spacecraft are different from typical terrestrial environments where smoke properties have been evaluated. It is critically important to detect a fire in its early phase before a flame is established, given the fixed volume of air on any spacecraft. Consequently, the primary target for spacecraft fire detection is pyrolysis products rather than soot. Experimental investigations have been performed at three different NASA facilities which characterize smoke aerosols from overheating common spacecraft materials. The earliest effort consists of aerosol measurements in low gravity, called the Smoke Aerosol Measurement Experiment (SAME), and subsequent ground-based testing of SAME smoke in 55-gallon drums with an aerosol reference instrument. Another set of experiments were performed at NASAs Johnson Space Center White Sands Test Facility (WSTF), with additional fuels and an alternate smoke production method. Measurements of these smoke products include mass and number concentration, and a thermal precipitator was designed for this investigation to capture particles for microscopic analysis. The final experiments presented are from NASAs Gases and Aerosols from Smoldering Polymers (GASP) Laboratory, with selected results focusing on realistic fuel preparations and heating profiles with regards to early detection of smoke. SAFFIRE is the upcoming large-scale fire experiment which will be executed in a Cygnus vehicle after it undocks from the ISS.

Aerosol↗

X ray microscope assembly and alignment support and advanced x ray microscope design and analysis

Considerable efforts have been devoted recently to the design, analysis, fabrication, and testing of spherical Schwarzschild microscopes for soft x ray application in microscopy and projection lithography. The spherical Schwarzschild microscope consists of two concentric spherical mirrors configured such that the third order spherical aberration and coma are zero. Since multilayers are used on the mirror substrates for x ray applications, it is desirable to have only two reflecting surfaces in a microscope. In order to reduce microscope aberrations and increase the field of view, generalized mirror surface profiles have been considered in this investigation. Based on incoherent and sine wave modulation transfer function (MTF) calculations, the object plane resolution of a microscope has been analyzed as a function of the object height and numerical aperture (NA) of the primary for several spherical Schwarzschild, conic, and aspherical head reflecting two mirror microscope configurations.

Shealy, David L.↗

Advanced water window x-ray microscope design and analysis

The project was focused on the design and analysis of an advanced water window soft-x-ray microscope. The activities were accomplished by completing three tasks contained in the statement of work of this contract. The new results confirm that in order to achieve resolutions greater than three times the wavelength of the incident radiation, it will be necessary to use aspherical mirror surfaces and to use graded multilayer coatings on the secondary (to accommodate the large variations of the angle of incidence over the secondary when operating the microscope at numerical apertures of 0.35 or greater). The results are included in a manuscript which is enclosed in the Appendix.

Shealy, D. L.↗

Acquisition of a High Resolution Field Emission Scanning Electron Microscope for the Analysis of Returned Samples

This grant furnished funds to purchase a state-of-the-art scanning electron microscope (SEM) to support our analytical facilities for extraterrestrial samples. After evaluating several instruments, we purchased a JEOL 6500F thermal field emission SEM with the following analytical accessories: EDAX energy-dispersive x-ray analysis system with fully automated control of instrument and sample stage; EDAX LEXS wavelength-dispersive x-ray spectrometer for high sensitivity light-element analysis; EDAX/TSL electron backscatter diffraction (EBSD) system with software for phase identification and crystal orientation mapping; Robinson backscatter electron detector; and an in situ micro-manipulator (Kleindiek). The total price was $550,000 (with $150,000 of the purchase supported by Carnegie institution matching funds). The microscope was delivered in October 2002, and most of the analytical accessories were installed by January 2003. With the exception of the wavelength spectrometer (which has been undergoing design changes) everything is working well and the SEM is in routine use in our laboratory.

Nittler, Larry R.↗

Determination of bulk diffusion lengths for angle-lapped semiconductor material via the scanning electron microscope: A theoretical analysis

A standard procedure for the determination of the minority carrier diffusion length by means of a scanning electron microscope (SEM) consists in scanning across an angle-lapped surface of a P-N junction and measuring the resultant short circuit current I sub sc as a function of beam position. A detailed analysis of the I sub sc originating from this configuration is presented. It is found that, for a point source excitation, the I sub sc depends very simply on x, the variable distance between the surface and the junction edge. The expression for the I sub sc of a planar junction device is well known. If d, the constant distance between the plane of the surface of the semiconductor and the junction edge in the expression for the I of a planar junction is merely replaced by x, the variable distance of the corresponding angle-lapped junction, an expression results which is correct to within a small fraction of a percent as long as the angle between the surfaces, 2 theta sub 1, is smaller than 10 deg.

Vonroos, O.↗

Design and analysis of multilayer x ray/XUV microscope

The design and analysis of a large number of normal incidence multilayer x ray microscopes based on the spherical mirror Schwarzschild configuration is examined. Design equations for the spherical mirror Schwarzschild microscopes are summarized and used to evaluate mirror parameters for microscopes with magnifications ranging from 2 to 50x. Ray tracing and diffraction analyses are carried out for many microscope configurations to determine image resolution as a function of system parameters. The results are summarized in three publication included herein. A preliminary study of advanced reflecting microscope configurations, where aspherics are used in place of the spherical microscope mirror elements, has indicated that the aspherical elements will improve off-axis image resolution and increase the effective field of view.

Shealy, David L.↗

Organic chemical analysis on a microscopic scale using two-step laser desorption/laser ionization mass spectrometry

The distribution of PAHs in the Allende meteorite has been measured using two-step laser desorption and laser multiphoton-ionization mass spectrometry. This method enables in situ analysis (with a spatial resolution of 1 mm or better) of selected organic molecules. Results show that PAH concentrations are locally high compared to the average concentration found by analysis of pulverized samples, and are found primarily in the fine-grained matrix; no PAHs were detected in the interiors of individual chondrules at the detection limit (about 0.05 ppm).

Kovalenko, L. J.↗

Ultra-high resolution water window x ray microscope optics design and analysis

This project has been focused on the design and analysis of an ultra-high resolution water window soft-x-ray microscope. These activities have been accomplished by completing two tasks contained in the statement of work of this contract. The new results from this work confirm: (1) that in order to achieve resolutions greater than three times the wavelength of the incident radiation, it will be necessary to use spherical mirror surfaces and to use graded multilayer coatings on the secondary in order to accommodate the large variations of the angle of incidence over the secondary when operating the microscope at numerical apertures of 0.35 or greater; (2) that surface contour errors will have a significant effect on the optical performance of the microscope and must be controlled to a peak-to-valley variation of 50-100 A and a frequency of 8 periods over the surface of a mirror; and (3) that tolerance analysis of the spherical Schwarzschild microscope has been shown that the water window operations will require 2-3 times tighter tolerances to achieve a similar performance of operations with 130 A radiation. These results have been included in a manuscript included in the appendix.

Shealy, David L.↗

First-order optical analysis of a quasi-microscope for planetary landers

A first-order geometrical optics analysis of a facsimile camera augmented with an auxiliary lens as magnifier is presented. This concept, called quasi-microscope, bridges the gap between surface resolutions of the order of 1 to 10 mm which can be obtained directly with planetary lander cameras and resolutions of the order of 0.2 to 10 microns which can be obtained only with relatively complex microscopes. A facsimile camera was considered in the analysis; however, the analytical results can also be applied to television and film cameras. It was found that quasi-microscope resolutions in the range from 10 to 100 microns are obtainable with current state-of-the-art lander facsimile cameras. For the Viking lander camera having an angular resolution of 0.04 deg, which was considered as a specific example, the best achievable resolution would be about 20 microns. The preferred approach to increase the resolution of the quasi-microscope would be, if possible, through an increase in angular resolution of the camera. A twofold to threefold improvement in resolution could also be achieved with a special camera focus position, but this approach tends to require larger and heavier auxiliary optics.

Huck, F. O.↗

Fractographic analysis of gaseous hydrogen induced cracking in 18Ni maraging steel

Electron microscope fractographic analysis supplemented an extensive study of the kinetics of gaseous hydrogen assisted cracking in 18Ni maraging steel. Temperature determined the crack path morphology in each steel which, in turn, was directly related to the temperature dependence of the crack growth rate. Crack growth in the low temperature regime proceeded along prior austenite grain boundaries. Increasing the temperature above a critical value produced a continuously increasing proportion of transgranular quasi-cleavage associated with lath martensite boundaries. The amount of transgranular cracking was qualitatively correlated with the degree of temperature-induced deviation from Arrhenius behavior. Fractographic observations are interpreted in terms of hypothesized mechanisms for gaseous hydrogen embrittlement. It is concluded that hydrogen segregation to prior austenite and lath martensite boundaries must be considered as a significant factor in developing mechanisms for gaseous embrittlement of high strength steels.

Gangloff, R. P.↗

NASA AMES Remote Operations Center for 2001

There is a Memorandum of Agreement between NASA Ames, JPL, West Virginia University and University of Arizona which led to funding for the MECA microscope and to the establishment of an Ames facility for science analysis of microscopic and other data. The data and analysis will be by agreement of the Mars Environmental Compatibility Assessment (MECA), Robotic Arm Camera (RAC) and other PI's. This facility is intended to complement other analysis efforts with one objective of this facility being to test the latest information technologies in support of actual mission science operations. Additionally, it will be used as a laboratory for the exploration of collaborative science activities. With a goal of enhancing the science return for both Human Exploration and Development of Space (HEDS) and Astrobiology we shall utilize various tools such as superresolution and the Virtual Environment Vehicle Interface (VEVI) virtual reality visualization tools. In this presentation we will describe the current planning for this facility.

Sims, M.↗

The Combined Detection of Morphological and Molecular Biomarkers: Implications for Astrobiology

Experience gathered by previous researchers during their hunt for evidence of early Earth life has shown the complexity in interpreting observations of possible microfossils and to establish the evidence to be positive. Similarly, the stillsimmering controversy on the nature of the nano-structures in Martian meteorite ALH84001 described by McKay et al. (1996) emphasizes the difficulties of conclusively identifying those structures as (a) fossilized bacterial cells and (b) establish their indigeneity. A better understanding of biological signatures in rocks is needed in order to identify traces of microbial life, which include morphological, mineralogical and chemical traces. It is thus considered crucial to tackle the problems emerging in the search for evidence of early life on Earth and in exopaleontological research with a multidisciplinary approach. With this is mind we applied surface sensitive Time of Flight-Secondary Ion Mass Spectroscopy (ToF-SIMS) to a previously described 25 m.y. old fossil bacterial biofilm. This technique allows in situ analysis with high mass resolution as well as molecular imaging of micron sized structures. As no extraction or derivatisation of the sample is required for ToF-SIMS analysis, electron microscopical investigation of the same samples subsequent to analysis is possible, thus allowing the combination of molecular and morphological biomarkers. The analysed fossil bacterial biofilms were associated with macrofossils from volcanoclastic lacustrine sediments from the Upper Oligocene Enspel formation (Germany). Preliminary scanning electron microscopy (SEM) studies have shown that a fossil structure interpreted as a coprolite purely consisted of fossilized bacterial biofilm. For ToF-SIMS investigation small particles were taken from the fossil biofilm and mounted onto Au-coated In-foil and analysed in a Phi Evans T-2000 TRIFT system. The ToF-SIMS analysed samples were Au/Pd-sputter coated and imaged using a Philips XL40 Field Emission Gun SEM (FEG-SEM). ToF-SIMS analysis of the organic rich fossil biofilm (TOC 29%) in the 0-100 Dalton (Da) range showed significant amounts of inorganic species, confirming the results obtained previously by EDX analysis, clearly showing the bacterial fossils to be mineralised. ToF-SIMS furthermore revealed the presence of a variety of low- and high-mass organic molecules and fragments thereof. These include peaks indicative of alkenes and alkanes, aromatic organic species and the polycyclic aromatic hydrocarbon naphthalene. More tentatively, peaks indicative of alkyl pyrroles and pyridyl-CH2 were identified. Other peaks of interest include peaks indicative of C(n)H(2n)O2 and C(n)H(2n-2)O2, which according to their general formula would suggest the presence of both saturated and unsaturated fatty acids although further in situ derivatisation experiments and GC-MS (Gas Chromatography MS) need to be applied to verify this beyond doubt. Furthermore, peaks at m/z 370, 384, 398, 412, 426, 440, 454 and 468 were identified, which indicate the potential presence of bacterial hopanes, a class of biomarkers indicative of bacteria. The main diagnostic peak for this group of chemicals is the fragment at m/z 191.18. Our studies conducted on purified hopane standards have shown that in the high-mass resolution mode differentiation of this diagnostic hopane peak and polyethylene at m/z 191.05 is possible. However, the spectra discussed here were collected in the lower resolution mapping mode, therefore this differentiation was not possible. The centroids of the possible hopane peaks obtained on the fossil biofilms are well within the range associated with bacterial hopanes. There is a strong possibility therefore that hopanoids may be associated with the fossil bacterial cells. Due to the non-destructive nature of ToF-SIMS, analysed samples can be studied using SEM, thus allowing the combination of morphological and molecular biomarkers. Subsequent SEM analysis of the ToF-SIMS analysed samples confirmed that the analysed material purely consists of fossil bacterial cells. This is thus the first successful effort to demonstrate the combination of spectral and morphological biomarkers. The advantages of highly sensitive non-destructive in situ analysis techniques for biomarker detection are invaluable, particularly with respect to envisaged Mars sample return missions, as it may allow us to identify remains and traces of former microbial life in both ancient terrestrial and extraterrestrial materials. This technique may prove particularly useful in the quest for extraterrestrial life with respect to precious extraterrestrial materials, as minute quantities are sufficient to conduct analysis.

Toporski, J.↗

Development of a miniature scanning electron microscope for in-flight analysis of comet dust

A description is presented of an instrument which was developed with the original goal of being flown on the International Comet Mission, scheduled for a 1985 launch. The Scanning Electron Microscope and Particle Analyzer (SEMPA) electron miniprobe is a miniaturized electrostatically focused electron microscope and energy dispersive X-ray analyzer for in-flight analysis of comet dust particles. It was designed to be flown on board a comet rendezvous spacecraft. Other potential applications are related to asteroid rendezvous and planetary lander missions. According to the development objectives, SEMPA miniprobe is to have the capability for imaging and elemental analysis of particles in the size range of 0.25 microns and larger.

Conley, J. M.↗