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Dynamics Impact Tolerance of Shuttle RCC Leading Edge Panels Using LS-DYNA

This paper describes a research program conducted to enable accurate prediction of the impact tolerance of the shuttle Orbiter leading-edge wing panels using physics-based codes such as LS-DYNA, a nonlinear, explicit transient dynamic finite element code. The shuttle leading-edge panels are constructed of Reinforced-Carbon-Carbon (RCC) composite material, which is used because of its thermal properties to protect the shuttle during reentry into the Earth's atmosphere. Accurate predictions of impact damage from insulating foam and other debris strikes that occur during launch required materials characterization of expected debris, including strain-rate effects. First, analytical models of individual foam and RCC materials were validated. Next, analytical models of foam cylinders impacting 6- in. x 6-in. RCC flat plates were developed and validated. LS-DYNA pre-test models of the RCC flat plate specimens established the impact velocity of the test for three damage levels: no-detectable damage, non-destructive evaluation (NDE) detectable damage, or visible damage such as a through crack or hole. Finally, the threshold of impact damage for RCC on representative Orbiter wing panels was predicted for both a small through crack and for NDE-detectable damage.

Fasanella, Edwin L.↗

Dynamic Impact Tolerance of Shuttle RCC Leading Edge Panels using LS-DYNA

This paper describes a research program conducted to enable accurate prediction of the impact tolerance of the shuttle Orbiter leading-edge wing panels using 'physics-based- codes such as LS-DYNA, a nonlinear, explicit transient dynamic finite element code. The shuttle leading-edge panels are constructed of Reinforced-Carbon-Carbon (RCC) composite material, which issued because of its thermal properties to protect the shuttle during re-entry into the Earth's atmosphere. Accurate predictions of impact damage from insulating foam and other debris strikes that occur during launch required materials characterization of expected debris, including strain-rate effects. First, analytical models of individual foam and RCC materials were validated. Next, analytical models of individual foam cylinders impacting 6-in. x 6-in. RCC flat plates were developed and validated. LS-DYNA pre-test models of the RCC flat plate specimens established the impact velocity of the test for three damage levels: no-detectable damage, non-destructive evaluation (NDE) detectable damage, or visible damage such as a through crack or hole. Finally, the threshold of impact damage for RCC on representative Orbiter wing panels was predicted for both a small through crack and for NDE-detectable damage.

Fasanella, Edwin↗

NASA Research Center Contributions to Space Shuttle Return to Flight (SSRTF)

Contributions provided by the NASA Research Centers to key Space Shuttle return-to-flight milestones, with an emphasis on debris and Thermal Protection System (TPS) damage characterization, are described herein. Several CAIB recommendations and Space Shuttle Program directives deal with the mitigation of external tank foam insulation as a debris source, including material characterization as well as potential design changes, and an understanding of Orbiter TPS material characteristics, damage scenarios, and repair options. Ames, Glenn, and Langley Research Centers have performed analytic studies, conducted experimental testing, and developed new technologies, analysis tools, and hardware to contribute to each of these recommendations. For the External Tank (ET), these include studies of spray-on foam insulation (SOFI), investigations of potential design changes, and applications of advanced non-destructive evaluation (NDE) technologies to understand ET TPS shedding during liftoff and ascent. The end-to-end debris assessment included transport analysis to determine the probabilities of impact for various debris sources. For the Orbiter, methods were developed, and validated through experimental testing, to determine thresholds for potential damage of Orbiter TPS components. Analysis tools were developed and validated for on-orbit TPS damage assessments, especially in the area of aerothermal environments. Advanced NDE technologies were also applied to the Orbiter TPS components, including sensor technologies to detect wing leading edge impacts during liftoff and ascent. Work is continuing to develop certified TPS repair options and to develop improved methodologies for reinforced carbon-carbon (RCC) damage progression to assist in on-orbit repair decision philosophy.

Cockrell, Charles E., Jr.↗

Assessment of Shape Memory Alloys - From Atoms To Actuators - Via In Situ Neutron Diffraction

As shape memory alloys (SMAs) become an established actuator technology, it is important to identify the fundamental mechanisms responsible for their performance by understanding microstructure performance relationships from processing to final form. Yet, microstructural examination of SMAs at stress and temperature is often a challenge since structural changes occur with stress and temperature and microstructures cannot be preserved through quenching or after stress removal, as would be the case for conventional materials. One solution to this dilemma is in situ neutron diffraction, which has been applied to the investigation of SMAs and has offered a unique approach to reveal the fundamental micromechanics and microstructural aspects of bulk SMAs in a non-destructive setting. Through this technique, it is possible to directly correlate the micromechanical responses (e.g., internal residual stresses, lattice strains), microstructural evolutions (e.g., texture, defects) and phase transformation properties (e.g., phase fractions, kinetics) to the macroscopic actuator behavior. In this work, in situ neutron diffraction was systematically employed to evaluate the deformation and transformation behavior of SMAs under typical actuator conditions. Austenite and martensite phases, yield behavior, variant selection and transformation temperatures were characterized for a polycrystalline NiTi (49.9 at. Ni). As the alloy transforms under thermomechanical loading, the measured textures and lattice plane-level variations were directly related to the cyclic actuation-strain characteristics and the dimensional instability (strain ratcheting) commonly observed in this alloy. The effect of training on the shape memory characteristics of the alloy and the development of two-way shape memory effect (TWSME) were also assessed. The final conversion from a material to a useful actuator, typically termed shape setting, was also investigated in situ during constrained heatingcooling and subsequent shape recovery experiments. Neutron diffraction techniques are also being applied to the investigation of novel high temperature SMAs with the objective of designing alloys with better stability, higher transition temperatures and ultimately superior durability.

Shape Memory Alloys↗

Creep and Environmental Durability of EBC/CMCs Under Imposed Thermal Gradient Conditions

Interest in SiC fiber-reinforced SiC ceramic matrix composite (CMC) environmental barrier coating (EBC) systems for use in high temperature structural applications has prompted the need for characterization of material strength and creep performance under complex aerospace turbine engine environments. Stress-rupture tests have been performed on SiC/SiC composites systems, with varying fiber types and coating schemes to demonstrate material behavior under isothermal conditions. Further testing was conducted under exposure to thermal stress gradients to determine the effect on creep resistance and material durability. In order to understand the associated damage mechanisms, emphasis is placed on experimental techniques as well as implementation of non-destructive evaluation; including electrical resistivity monitoring. The influence of environmental and loading conditions on life-limiting material properties is shown.

Appleby, Matthew↗

An Evanescent Microwave Probe for Super-Resolution Nondestructive Imaging of Metals, Semiconductors, Dielectrics, Composites and Biological Specimens

Using evanescent microwaves with decay lengths determined by a combination of microwave wavelength (lambda) and waveguide termination geometry, we have imaged and mapped material non-uniformities and defects with a resolving capability of lambda/3800=79 microns at 1 GHz. In our method a microstrip quarter wavelength resonator was used to generate evanescent microwaves. We imaged materials with a wide range of conductivities. Carbon composites, dielectrics (Duroid, polymers), semiconductors (3C-SiC, polysilicon, natural diamond), metals (tungsten alloys, copper, zinc, steel), high-temperature superconductors, and botanical samples were scanned for defects, residual stresses, integrity of brazed junctions, subsurface features, areas of different film thickness and moisture content. The evanescent microwave probe is a versatile tool and it can be used to perform very fast, large scale mapping of a wide range of materials. This method of characterization compares favorably with ultrasound testing, which has a resolution of about 0.1 mm and suffers from high absorption in composite materials and poor transmission across boundaries. Eddy current methods which can have a resolution on the order of 50 microns are restricted to evaluating conducting materials. Evanescent microwave imaging, with careful choice of operating frequency and probe geometry, can have a resolution of up to 1 micron. In this method we can scan hot and moving objects, sample preparation is not required, testing is non-destructive, non-invasive and non-contact, and can be done in air, in liquid or in vacuum.

Pathak, P. S.↗

Identification of New Lithic Clasts in Lunar Breccia 14305 by Micro-CT and Micro-XRF Analysis

From 1969 to 1972, Apollo astronauts collected 382 kg of rocks, soils, and core samples from six locations on the surface of the Moon. The samples were initially characterized, largely by binocular examination, in a custom-built facility at Johnson Space Center (JSC), and the samples have been curated at JSC ever since. Despite over 40 years of study, demand for samples remains high (~500 subsamples per year are allocated to scientists around the world), particularly for plutonic (e.g., anorthosites, norites, etc.) and evolved (e.g., granites, KREEP basalts) lithologies. The reason for the prolonged interest is that as new scientists and new techniques examine the samples, our understanding of how the Moon, Earth, and other inner Solar System bodies formed and evolved continues to grow. Scientists continually clamor for new samples to test their emerging hypotheses. Although all of the large Apollo samples that are igneous rocks have been classified, many Apollo samples are complex polymict breccias that have previously yielded large (cm-sized) igneous clasts. In this work we present the initial efforts to use the non-destructive techniques of micro-computed tomography (micro-CT) and micro x-ray fluorescence (micro-XRF) to identify large lithic clasts in Apollo 14 polymict breccia sample 14305. The sample in this study is 14305,483, a 150 g slab of regolith breccia 14305 measuring 10x6x2 cm (Figure 1a). The sample was scanned at the University of Texas High-Resolution X-ray CT Facility on an Xradia MicroXCT scanner. Two adjacent overlapping volumes were acquired at 49.2 micrometer resolution and stitched together, resulting in 1766 slices. Each volume was acquired at 100 kV accelerating voltage and 98 mA beam current with a 1 mm CaF2 filter, with 2161 views gathered over 360deg at 3 seconds acquisition time per view. Micro-XRF analyses were done at Washington University in St. Louis, Missouri on an EDAX Orbis PC micro-XRF instrument. Multiple scans were made at 40 kV accelerating voltage, 800 mA beam current, 30 μm beam diameter, and a beam spacing of 30-120 micrometer. The micro-CT scan of 14305,483 (Figure 2) was able to identify several large lithic clasts (approx. 1 cm) within the interior of the slab. These clasts will be exposed by band-sawing or chipping of the slab, and their composition more fully characterized by subsequent micro-XRF analysis. In addition to lithic clasts, the micro-CT scans identified numerous mineral clasts, including many FeNi metal grains, as well as the prominent fractures within the slab. The micro-XRF analyses (Figure 1b,c) of the slab surfaces revealed the bulk chemical compositions (qualitative) of the different clast types observed. In particular, by looking at the ratios of major elements (e.g. Ca:Mg:Fe), differences among the many observed clast types are readily observed. Moreover, several clasts not apparent to the naked eye were revealed in the K:Al:Si ratio map. The scans are also able to identify small grains of Zr- and P-rich minerals (not shown), which could in turn yield important age dates for the samples.

Zeigler, Ryan A.↗

Error analysis of leaf area estimates made from allometric regression models

Biological net productivity, measured in terms of the change in biomass with time, affects global productivity and the quality of life through biochemical and hydrological cycles and by its effect on the overall energy balance. Estimating leaf area for large ecosystems is one of the more important means of monitoring this productivity. For a particular forest plot, the leaf area is often estimated by a two-stage process. In the first stage, known as dimension analysis, a small number of trees are felled so that their areas can be measured as accurately as possible. These leaf areas are then related to non-destructive, easily-measured features such as bole diameter and tree height, by using a regression model. In the second stage, the non-destructive features are measured for all or for a sample of trees in the plots and then used as input into the regression model to estimate the total leaf area. Because both stages of the estimation process are subject to error, it is difficult to evaluate the accuracy of the final plot leaf area estimates. This paper illustrates how a complete error analysis can be made, using an example from a study made on aspen trees in northern Minnesota. The study was a joint effort by NASA and the University of California at Santa Barbara known as COVER (Characterization of Vegetation with Remote Sensing).

Feiveson, A. H.↗

Composite Material Property Nondestructive Characterization Using Obliquely Insonified Ultrasonic Waves

The analysis of reflected ultrasonic waves induced by oblique insonification of composite materials is a powerful tool for providing informations about defects and material properties. A device was developed to manipulate a pair of transmitting and receiving transducers at vrious angles of wave incidence and propagation with the fiber orientation.

Non-Destructive Evaluation Composites Mechanical P↗

Mars Observer Propulsion and Pyrotechnics Corrective Actions Test Program Status-1999

An extensive propulsion and pyrotechnic test program has been in progress at the NASA White Sands Test Facility since 1995. This program created the capabilities to: accurately measure and characterize pyrovalve combustion product blow-by into propellant systems; characterize valve operation using a Velocity Interferometer System for Any Reflector (VISAR); and evaluate hydrazine and monomethylhydrazine thermal decomposition initiated by blow-by. These capabilities were further utilized and refined this year. Low blow-by pyrovalves manufactured by Conax Florida Corporation continued to be evaluated as a potential corrective measure for blow-by induced propellant explosions. Development and testing of various advanced pyrovalves and investigation of explosion mechanisms also continued. Current and near-term testing includes: evaluation of 3/8 in. Conax pyrovalves and other commercially available valves; development and testing of advanced pyrovalve subcomponent technologies including a zero blow-by pyrovalve ram, composite overwrapped ram cylinder, and a zero particulate generating poppet; investigation of non-destructive evaluation techniques to evaluate pyrovalve ram seals; and testing and modeling of pyrotechnically induced explosive hydrazine decomposition. Evaluation of 3/8 in. Conax valves will include operational margin testing to be accomplished at NASA Langley Research Center. The test program also seeks to compile and format significant amounts of data from this and other pyrovalve test programs to generate a pyrovalve applications handbook. The handbook will facilitate formation of standards that ensure safe spacecraft applications. Current data and future plans are discussed, and community interaction is encouraged.

Saulsberry, Regor↗

Fabrication and Characterization of Diffusion Bonds for Silicon Carbide

Diffusion bonds of silicon carbide (SiC) were fabricated using several different types of titanium (Ti) based interlayers between the SiC substrates. The interlayers were an alloyed Ti foil, a pure Ti foil, and a physically vapor deposited (PVD) Ti coating. Microscopy was conducted to evaluate the cross-sections of the resulting bonds. Microprobe analysis identified reaction formed phases in the diffusion bonded region. Uniform and well adhered bonds were formed between the SiC substrates. In the case where the alloyed Ti foil or a thick Ti coating (i.e. 20 micron) was used as the interlayer, microcracks and several phases were present in the diffusion bonds. When a thinner interlayer was used (i.e. 10 micron PVD Ti), no microcracks were observed and only two reaction formed phases were present. The two phases were preferred and fully reacted phases that did not introduce thermal stresses or microcracks during the cool-down stage after processing. Diffusion bonded samples were evaluated with the non-destructive evaluation (NDE) methods of pulsed thermography and immersion ultrasonic testing. Joined SiC substrates that were fully bonded and that had simulated bond flaws in the interlayer were also evaluated using immersion ultrasound. Pull testing was conducted on the bonds to determine the tensile strength. To demonstrate the joining approach for a complex multilayered component for a low NOx injector application, the diffusion bonding approach was used to join three 4" diameter SiC discs that contained complex fuel and air flow channels.

Halbig, Michael↗

A New Look at Aubrites: Investigating 3D Modal Mineralogy with X-Ray Computed Tomography

The aubrites (approximately 30 known meteorites) are a unique group of differentiated meteorites that formed on asteroids with oxygen fugacities (ƒO2) from approximately 2 to approximately 6 log units below the iron-wustite buffer. At these highly reduced conditions, elements deviate from the geochemical behavior exhibited at terrestrial ƒO2, forming FeO-poor silicates and exotic sulfides. While previous studies have described the petrology and 2D modal abundances of aubrites, this work investigates the 3D modal mineralogies of silicate, metal, and sulfide phases in aubrite samples, which are then compared to the available 2D data. In addition to 3D modal mineralogies, we have examined the geochemistry of fourteen aubrites, including mineral major-element compositions, bulk-rock compositions, and oxygen isotopic compositions to understand their formation and evolution at extreme ƒO2 conditions. We utilize X-ray computed tomography (XCT) to non-destructively analyze the distribution and abundances of mineral phases in aubrites and locate composite clasts of sulfide grains for future analytical study. In order to better constrain elemental behavior under reduced conditions, we specifically target minerals phases that comprise moderately volatile elements (i.e. oldhamite [CaS], caswellsilverite [NaCrS2] and djerfisherite [K6Na(Fe,Cu,Ni)25S26Cl]) as it has been shown that their geochemical behavior changes as a function of ƒO2. Currently, we have produced 3D scans of the Norton County aubrite. The results of the XCT data have allowed for the determination of the abundances of silicate groundmass (i.e., enstatite, forsterite, albite, and diopside), light (based on electron density) sulfides (i.e. alabandite [MnS] and daubréelite [FeCr2S4]), heavy (based on electron density) sulfides (i.e., troilite [FeS]), and Fe,Ni metal by segmenting a density histogram in Volume Graphics Studio software. XCT scans of additional aubrites are underway. By combining the 3D representation of the exotic phases found in aubrites with existing 2D characterizations, we are able to better determine modal abundances. By integrating 3D and 2D modal abundances and geochemistry, we can ultimately better constrain aubrite petrogenesis and elemental partitioning under reduced conditions. Furthermore, application of this new 3D approach offers the opportunity to identify and select clasts for future study prior to cutting the sample, which will minimize sample loss of this precious material.

Wilbur, Zoe↗

Use of Raman Spectroscopy and Delta Volume Growth from Void Collapse to Assess Overwrap Stress Gradients Compromising the Reliability of Large Kevlar/Epoxy COPVs

Composite Overwrapped Pressure Vessels (COPVs) are frequently used for storing pressurized gases aboard spacecraft and aircraft when weight saving is desirable compared to all-metal versions. Failure mechanisms in fibrous COPVs and variability in lifetime can be very different from their metallic counterparts; in the former, catastrophic stress-rupture can occur with virtually no warning, whereas in latter, a leak before burst design philosophy can be implemented. Qualification and certification typically requires only one burst test on a production sample (possibly after several pressure cycles) and the vessel need only meet a design burst strength (the maximum operating pressure divided by a knockdown factor). Typically there is no requirement to assess variability in burst strength or lifetime, much less determine production and materials processing parameters important to control of such variability. Characterizing such variability and its source is crucial to models for calculating required reliability over a given lifetime (e.g. R = 0.9999 for 15 years). In this paper we present a case study of how lack of control of certain process parameters in COPV manufacturing can result in variations among vessels and between production runs that can greatly increase uncertainty and reduce reliability. The vessels considered are 40-inch ( NASA Glenn Research center, Cleveland, OH, 44135 29,500 in3 ) spherical COPVs with a 0.74 in. thick Kevlar49/epoxy overwrap and with a titanium liner of which 34 were originally produced. Two burst tests were eventually performed that unexpectedly differed by almost 5%, and were 10% lower than anticipated from burst tests on 26-inch sister vessels similar in every detail. A major observation from measurements made during proof testing (autofrettage) of the 40-inch vessels was that permanent volume growth from liner yielding varied by a factor of more than two (150 in3 to 360 in3 ), which suggests large differences in the residual stress gradient through their overwraps. This resulted in large uncertainty in true fiber stress ratio (fiber stress at operating pressure divided by fiber stress at burst) which governs lifetime. The vessels were originally designed with tight safety margins, so it became crucial to develop a non-destructive evaluation (NDE) technique to directly measure the overwrap residual stress state of each vessel, and to identify those vessels at highest risk of having poor reliability. This paper describes a Raman Spectroscopy technique for measuring certain patterns of fluctuation in fiber elastic strains over the outside vessel surface (where all but one wrap is exposed at certain locations) that are shown to directly correlate to increased fiber stress ratios and reduced reliability.

Kezirian, Michael T.↗

Using Technology to Better Characterize the Apollo Sample Suite: A Retroactive PET Analysis and Potential Model for Future Sample Return Missions

From 1969-1972 the Apollo missions collected 382 kg of lunar samples from six distinct locations on the Moon. Studies of the Apollo sample suite have shaped our understanding of the formation and early evolution of the Earth-Moon system, and have had important implications for studies of the other terrestrial planets (e.g., through the calibration of the crater counting record) and even the outer planets (e.g., the Nice model of the dynamical evolution of the Solar System). Despite nearly 50 years of detailed research on Apollo samples, scientists are still developing new theories about the origin and evolution of the Moon. Three areas of active research are: (1) the abundance of water (and other volatiles) in the lunar mantle, (2) the timing of the formation of the Moon and the duration of lunar magma ocean crystallization, (3) the formation of evolved lunar lithologies (e.g., granites) and implications for tertiary crustal processes on the Moon. In order to fully understand these (and many other) theories about the Moon, scientists need access to "new" lunar samples, particularly new plutonic samples. Over 100 lunar meteorites have been identified over the past 30 years, and the study of these samples has greatly aided in our understanding of the Moon. However, terrestrial alteration and the lack of geologic context limit what can be learned from the lunar meteorites. Although no "new" large plutonic samples (i.e., hand-samples) remain to be discovered in the Apollo sample collection, there are many large polymict breccias in the Apollo collection containing relatively large (approximately 1 cm or larger) previously identified plutonic clasts, as well as a large number of unclassified lithic clasts. In addition, new, previously unidentified plutonic clasts are potentially discoverable within these breccias. The question becomes how to non-destructively locate and identify new lithic clasts of interest while minimizing the contamination and physical degradation of the samples.

Zeigler, R. A.↗

Use of Computed Tomography for Characterizing Materials Grown Terrestrially and in Microgravity

Computed Tomography (CT) has advanced considerably since being responsible for such dramatic advances in diagnostics within the medical field. It has become a major tool in non destructive evaluation (NDE), and is used in many fields as diverse as coal-mining to metal solidification to examination of rock cores. A review of industrial applications has been written by Dennis. It is only recently that the technique has been seriously used to determine composition through precise measurement of density. While such applications are restricted to cases when there is no ambiguity in the relationship of composition to density. Thus alloy solid solutions lend themselves to compositional analysis provided there is a large change in density with composition. The technique is most useful when rapid non-destructive evaluation is needed. Such cases will occur with samples returning from the International Space Station (ISS) when knowledge of the results could affect future strategies for processing of on-board samples. Experiments from those Principal Investigators (PI) that are most likely to benefit from early CT scanning are discussed. With a dearth of samples, the major emphasis in the first part of this project has been on preparing suitable standards, optimizing the CT technique for these applications, and using the CT system to determine density variations with temperature. An interesting application of CT has been in the examination of meteorites, which can be classified as space-grown materials and will certainly have solidified in a low gravity environment.

Gillies, Donald C.↗

Numerical Modeling, Thermomechanical Testing, and NDE Procedures for Prediction of Microcracking Induced Permeability of Cryogenic Composites

Reusable Space Vehicles will include light cryogenic composite fuel tanks that must not leak excessively even after multiple launches. Damage in cryogenic composite fuel tanks induced during manufacturing and advanced by thermomechanical cycling can accelerate leakage of the propellant. Whether the leakage exceeds tolerable levels depends on many factors, including pressure gradients, microcrack density, other damage such as delamination, connectivity of the cracks, residual stresses from manufacture, service-induced stresses from thermal and mechanical loads, and composite lay-up. Although it is critical to experimentally characterize permeability during various thermal and mechanical load histories, optimal design depends on having analytical models that can predict the effect of various parameters on performance. Our broad goal is to develop such models that are experimentally validated by destructive and non-destructive evaluation means.

Noh, Jae↗

Preliminary Examination of the Interstellar Collector of Stardust

The findings of the Stardust spacecraft mission returned to earth in January 2006 are discussed. The spacecraft returned two unprecedented and independent extraterrestrial samples: the first sample of a comet and the first samples of contemporary interstellar dust. An important lesson from the cometary Preliminary Examination (PE) was that the Stardust cometary samples in aerogel presented a technical challenge. Captured particles often separate into multiple fragments, intimately mix with aerogel and are typically buried hundreds of microns to millimeters deep in the aerogel collectors. The interstellar dust samples are likely much more challenging since they are expected to be orders of magnitudes smaller in mass, and their fluence is two orders of magnitude smaller than that of the cometary particles. The goal of the Stardust Interstellar Preliminary Examination (ISPE) is to answer several broad questions, including: which features in the interstellar collector aerogel were generated by hypervelocity impact and how much morphological and trajectory information may be gained?; how well resolved are the trajectories of probable interstellar particles from those of interplanetary origin?; and, by comparison to impacts by known particle dimensions in laboratory experiments, what was the mass distribution of the impacting particles? To answer these questions, and others, non-destructive, sequential, non-invasive analyses of interstellar dust candidates extracted from the Stardust interstellar tray will be performed. The total duration of the ISPE will be three years and will differ from the Stardust cometary PE in that data acquisition for the initial characterization stage will be prolonged and will continue simultaneously and parallel with data publications and release of the first samples for further investigation.

Westphal, A. J.↗

Application of CO2 Snow Jet Cleaning in Conjunction with Laboratory Based Total Reflection X-Ray Fluorescence

The Genesis mission was the first mission returning solar material to Earth since the Apollo program [1,2]. Unfortunately the return of the space craft on September 8, 2004 resulted in a crash landing, which shattered the samples into small fragments and exposed them to desert soil and other debris. Thus only small fragments of the original collectors are available, each having different degrees of surface contamination. Thorough surface cleaning is required to allow for subsequent analysis of solar wind material embedded within. An initial cleaning procedure was developed in coordination with Johnson Space Center which focused on removing larger sized particulates and a thin film organic contamination acquired during collection in space [3]. However, many of the samples have additional residues and more rigorous and/or innovative cleaning steps might be necessary. These cleaning steps must affect only the surface to avoid leaching and re-distribution of solar wind material from the bulk of the collectors. To aid in development and identification of the most appropriate cleaning procedures each sample has to be thoroughly inspected before and after each cleaning step. Laboratory based total reflection X-ray fluorescence (TXRF) spectrometry lends itself to this task as it is a non-destructive and surface sensitive analytical method permitting analysis of elements from aluminum onward present at and near the surface of a flat substrate [4]. The suitability of TXRF has been demonstrated for several Genesis solar wind samples before and after various cleaning methods including acid treatment, gas cluster ion beam, and CO2 snow jet [5 - 7]. The latter one is non-invasive and did show some promise on one sample [5]. To investigate the feasibility of CO2 snow jet cleaning further, several flown Genesis samples were selected to be characterized before and after CO2 snow application with sample 61052 being discussed below.

Schmeling, M.↗