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NASA NTRS2019

Electron Beam Damage in Apatite: Limitations for SKα Measurements of S6+/∑S

In magmatic systems, the availabil- ity of excess oxygen that can react with multivalent elements such as Fe and S to change their charge (oxi- dation of Fe2+ to Fe3+ or reduction of S6+ to S2-) is characterized by a parameter called the oxygen fugacity (ƒO2). The ƒO2 controls the availability of these ions and consequently the minerals—and the chemistry of those minerals—that crystallize from a melt. Mineral mode and chemistry control how magmas evolve, and given that ƒO2 varies by many orders of magnitude on different planets [2], understanding the ƒO2 of a mag- ma is critical to relating observations about a magma to the body on which it forms. The mineral apatite was long thought to only incor- porate S6+ in a coupled substitution for P5+, but recently natural apatites with S2- were identified in lunar mare basalts that crystallized at low ƒO2 [3]. This suggests that apatite can be used as a monitor of ƒO2 assuming that one can 1) measure S6+/∑S (S6+ over total sulfur), and 2) determine some partitioning relationship be- tween apatite and melt for S6+ and S2-. The most common method for measuring S6+/∑S is X-ray Absorption Near-Edge Spectroscopy (XANES), but given the limited access to synchrotron facilities, it is wise to explore the potential of other methods for measuring S6+/∑S. One such possible method relies upon the shift in energy of the sulfur K-α peak on the electron microprobe. However, apatite is subject to well-documented beam damage [4, 5], so it is neces- sary to evaluate under what conditions can reliable S6+ ethod.

de Chizelle, J. Kuhn↗

NASA NTRS2011

FTIR Analysis of Aerogel Keystones from the Stardust Interstellar Dust Collector: Assessment of Terrestrial Organic Contamination and X-Ray Microprobe Beam Damage

The Stardust Interstellar Dust Collector (SIDC) was intended to capture and return contemporary interstellar dust. The approx.0.1 sq m collector was composed of aerogel tiles (85% of the collecting area) and aluminum foils and was exposed to the interstellar dust stream for a total exposure factor of 20 sq m day. The Stardust Interstellar Preliminary Examination (ISPE) is a consortium-based project to characterize the collection using nondestructive techniques. Sandford et al. recently assessed numerous potential sources of organic contaminants in the Stardust cometary collector. These contaminants could greatly complicate the analysis and interperetation of any organics associated with interstellar dust, particularly because signals from these particles are expected to be exceedingly small. Here, we present a summary of FTIR analyses of over 20 aerogel keystones, many of which contained candidates for interstellar dust.

Zolensky, M. E.↗

NASA NTRS1988

Characterization of electron-beam induced damage structures in natural fluorite, CaF2, by analytical electron microscopy

This paper describes the damage structure induced in natural CaF2 by the electron beam when using TEM. The observed 10-20 nm periodic features with coherent fringe patterns and the pronounced loss of fluorine found after the TEM exposure of 100-line-oriented and 111-oriented sections of CaF2 provides support for the mechanism of damage by decomposition of CaF2 into 2F and Ca, with the Ca precipitates maintaining a close topotaxial relationship with the parent CaF2.

Blake, D. F.↗

NASA NTRS1990

Electron beam induced damage in PECVD Si3N4 and SiO2 films on InP

Phosphorus rich plasma enhanced chemical vapor deposition (PECVD) of silicon nitride and silicon dioxide films on n-type indium phosphide (InP) substrates were exposed to electron beam irradiation in the 5 to 40 keV range for the purpose of characterizing the damage induced in the dielectic. The electron beam exposure was on the range of 10(exp -7) to 10(exp -3) C/sq cm. The damage to the devices was characterized by capacitance-voltage (C-V) measurements of the metal insulator semiconductor (MIS) capacitors. These results were compared to results obtained for radiation damage of thermal silicon dioxide on silicon (Si) MOS capacitors with similar exposures. The radiation induced damage in the PECVD silicon nitride films on InP was successfully annealed out in an hydrogen/nitrogen (H2/N2) ambient at 400 C for 15 min. The PECVD silicon dioxide films on InP had the least radiation damage, while the thermal silicon dioxide films on Si had the most radiation damage.

Pantic, Dragan M.↗

NASA NTRS1989

Electron-beam induced damage in thin insulating films on compound semiconductors

Phosphorus rich plasma enhanced chemical vapor deposition (PECVD) of silicon nitride and silicon dioxide films on n-type indium phosphide (InP) substrates were exposed to electron-beam irradiation in the 5 to 40 keV range for the purpose of characterizing the damage induced in the dielectric. The electron-beam exposure was on the range of 10(exp -7) to 10(exp -3) C/sq cm. The damage to the devices was characterized by capacitance-voltage (C-V) measurements of the metal insulator semiconductor (MIS) capacitors. These results were compared to results obtained for radiation damage of thermal silicon dioxide on silicon (Si) MOS capacitors with similar exposures. The radiation induced damage in the PECVD silicon nitride films on InP was successfully annealed out in an hydrogen/nitrogen (H2/N2) ambient at 400 C for 15 min. The PECVD silicon dioxide films on InP had the least radiation damage, while the thermal silicon dioxide films on Si had the most radiation damage.

Pantic, Dragan M.↗

NASA NTRS2018

Novel Applications of Focused Ion Beam Technique for Planetary Sample Analyses

We are using innovative FIB techniques to prepare samples of planetary materials for different types of coordinated analyses using ion microprobes, synchrotron beamlines, and specialized transmission electron microscopy (TEM) techniques. In these cases, the FIB sample preparation is the critical step in enabling these specialized analyses. We discuss several examples below utilizing the FEI Quanta3D instrument at the NASA Johnson Space Center. Trace element analyses utilizing synchrotron x-ray fluorescence. The trace element content of mineral grains in comet dust provides important clues on their formation and processing in the early solar system. We preformed coordinated analyses of a comet dust particle that had been prepared using ultramicrotomy for TEM analysis. Following the TEM analyses, we extracted a 70 nm thick section from a region of the carbon (C) film of the TEM grid, for additional analyses. A carbon ring ~2-3 μm thick was deposited on top of the C film using the FIB. The C film on the outer rim of the ring was milled away using various patterns to uniformly release the stresses on the film, preventing rupture and collapse, and was attached to the micromanipulator needle. We then isolated the ring completely and transferred the section to a silicon sample holder for analysis using the HXN (hard X-ray nanoprobe) beamline at NSLSII at Brookhaven National Lab. Coordinated Analyses of Presolar Grains. Rare sub-m presolar grains that originate in evolved stars and supernovae, occur in primitive astromaterials and are identified by their exotic isotopic compositions. Coordinated analyses of these grains using NanoSIMS, TEM, and other techniques on the same grain is enabled by innovative FIB sample preparation. In order to obtain subsequent isotopic analyses of Mg and Fe, contributions from surrounding grains were minimized. We precisely deposited a protective cap of Pt on top of the grain to preserve the grain of interest and then milled away about 5 μm diameter of the surrounding material. Following the isotopic analyses, the spindle was extracted and thinned to electron transparency for TEM microstructural analyses. In situ heating TEM experiments on lunar samples. We extracted a FIB thin section from Apollo 17 lunar rock 76015. To avoid ion-beam damage, e-beam deposition was used to deposit the first 500 nm of the C strap, followed by ion beam-assisted deposition of ~3 μm carbon. We performed an ex situ lift-out of the section and placed the section on one of the elements of a microelectromechanical systems (MEMS) - specialized heating substrate and attached the section to the substrate by depositing small C straps with the FIB. The heating chips utilize silicon nitride windows to support the samples and provide uniform heating while enabling TEM imaging. The heating chip was loaded into a Hitachi “Blaze” heating holder and analyzed using a Hitachi HF5000 at the University of Arizona.

Rahman, Z.↗

NASA NTRS1981

Electron beam induced damage in ITO coated Kapton

Data for the stability of thin conductive indium tin oxide films on 0.003 inch thick Kapton substrates during exposure of the surface to electron beams are reported. The electron beam energy was 3 keV and the diameter was about 0.8 mm. Thermal effects and surface modifications are considered. For primary current greater than 0.6 microamperes, an obvious dark discoloration with diameter approximately that of the beam was produced. The structure of the discolored region was studied with the scanning electron microscope, and the findings are stated. Surface modifications were explored by AES, obtaining spectra and secondary emission coefficient as a function of time for different beam intensities. In all cases beam exposure results in a decrease of the secondary yield but because of thermal effects this change, as well as composition changes, cannot be directly interpreted in terms of electron beam dosage.

Krainsky, I.↗

NASA NTRS1998

Potential for Fabric Damage by Welding Electron Beam

Welding electron beam effects on Nextel AF-62 ceramic fabric enable a preliminary, tentative interpretation of electron beam fabric damage. Static surface charging does not protect fabric from beam penetration, but penetration occurs only after a delay time. The delay time is thought to be that required for the buildup of outgassing products at the fabric surface to a point where arcing occurs. Extra long delays are noted when the gun is close enough to the surface to be shut off by outgassing emissions. Penetration at long distances is limited by beam attenuation from electronic collisions with the chamber atmosphere.

Fragomeni, James M.↗

NASA NTRS1992

Electron spectroscopy analysis

The Surface Science Laboratories at the University of Alabama in Huntsville (UAH) are equipped with x-ray photoelectron spectroscopy (XPS or ESCA) and Auger electron spectroscopy (AES) facilities. These techniques provide information from the uppermost atomic layers of a sample, and are thus truly surface sensitive. XPS provides both elemental and chemical state information without restriction on the type of material that can be analyzed. The sample is placed into an ultra high vacuum (UHV) chamber and irradiated with x-rays which cause the ejection of photoelectrons from the sample surface. Since x-rays do not normally cause charging problems or beam damage, XPS is applicable to a wide range of samples including metals, polymers, catalysts, and fibers. AES uses a beam of high energy electrons as a surface probe. Following electronic rearrangements within excited atoms by this probe, Auger electrons characteristic of each element present are emitted from the sample. The main advantage of electron induced AES is that the electron beam can be focused down to a small diameter and localized analysis can be carried out. On the rastering of this beam synchronously with a video display using established scanning electron microscopy techniques, physical images and chemical distribution maps of the surface can be produced. Thus very small features, such as electronic circuit elements or corrosion pits in metals, can be investigated. Facilities are available on both XPS and AES instruments for depth-profiling of materials, using a beam of argon ions to sputter away consecutive layers of material to reveal sub-surface (and even semi-bulk) analyses.

Gregory, John C.↗

NASA NTRS1990

An examination of impact damage in glass-phenolic and aluminum honeycomb core composite panels

An examination of low velocity impact damage to glass-phenolic and aluminum core honeycomb sandwich panels with carbon-epoxy facesheets is presented. An instrumented drop weight impact test apparatus was utilized to inflict damage at energy ranges between 0.7 and 4.2 joules. Specimens were checked for extent of damage by cross sectional examination. The effect of core damage was assessed by subjecting impact-damaged beams to four-point bend tests. Skin-only specimens (facings not bonded to honeycomb) were also tested for comparison purposes. Results show that core buckling is the first damage mode, followed by delaminations in the facings, matrix cracking, and finally fiber breakage. The aluminum honeycomb panels exhibited a larger core damage zone and more facing delaminations than the glass-phenolic core, but could withstand more shear stress when damaged than the glass-phenolic core specimens.

Nettles, A. T.↗

NASA NTRS2012

Coordinated STEM/FIB/NanoSIMS Analyses of Presolar Silicates in Comet Dust and Primitive Meteorites

Silicate grains were among the most abundant mineralogical building blocks of our Solar System. These grains were the detritus from earlier generations of stars that have been recycled in the early solar nebula. Rare sub-micrometer survivors of this processing have been identified in meteorites, micrometeorites and interplanetary dust particles (IDPs). These silicate grains are recognized as presolar in origin because of their extremely anomalous isotopic compositions that reflect nucleosynthetic processes in their stellar sources (evolved stars, novae and supernovae). We perform coordinated chemical, mineralogical and isotopic studies of these grains to determine their origins and histories. We examine the complex mineralogy and petrography of presolar silicates using imaging, diffraction and chemical data obtained from thin sections with the JSC JEOL 2500 field-emission STEM equipped with a Noran thin window energy dispersive x-ray (EDX) spectrometer and a Gatan Tridiem GIF. Quantitative element x-ray maps (spectrum images) are acquired by rastering a 4 nm incident probe whose dwell time is minimized to avoid beam damage and element diffusion during mapping. Successive image layers are acquired and combined in order to achieve approx 1% counting statistics for major elements. The IDP samples are prepared by ultramicrotomy of particles embedded in epoxy or elemental sulfur. After EDX mapping, the sections are subjected to C, N, and O isotopic imaging with the JSC NanoSIMS 50L ion microprobe. We prepare sections of some meteorite grains using the JSC FEI Quanta 3D focused ion beam (FIB) instrument. The specimen surface is protected from the FIB milling process by layers of electron beam-deposited C and Pt followed by an ion-deposited Pt layer. We also use the FIB to preferentially remove surrounding grains to reduce the background in subsequent NanoSIMS measurements. For mineralogical studies, we again employ the FIB instrument to deposit a protective cap over the grain of interest and then extract the grain and thin it to electron transparency for TEM analysis.

Keller, Lindsay↗

NASA NTRS1990

A probe for real-time images of particle beams and their analyses in a merged-beams apparatus

A real-time charged particle beam probe was developed, which can be used both as a beam diagnostic (beam tuning) and to quantitatively determine the three-dimensional density distribution of a beam. The probe consists of a microchannel plate, an aluminized phosphor screen deposited on a fiber-optic faceplate, a flexible fiber-optic bundle, and a charge injection device (CID) in tandem. Digital or analog video output of the CID is fed into a computer or oscilloscope, respectively, for analysis or observation. The probe can be moved continuously along the beams' paths to obtain 'pictures' of the beam at any desired interval, thus giving three-dimensional form factors. The beams, singly or simultaneously, may be observed on the monitor facilitating the task of beam adjustment for optimum overlap. The digital output is used for quantitative computation of the beam overlaps. The device is linear with beam intensity, but the performance degrades with time due to beam damage of the microchannel plate.

Forand, J. L.↗

NASA NTRS1992

Optical and TEM study of shock metamorphism from the Sedan test site

Thus far, detailed petrologic studies of shock metamorphism have been performed on samples recovered from laboratory experiments and on a few natural impactites. The loading history of these samples is quite different: In particular, laboratory experiments spend only a short time (less than 1 microsec) at peak pressure, whereas natural impactites may have stress pulses from 0.1 - 1 ms. On the other hand, laboratory experiments have known stress histories; natural impactites do not. Natural samples are also subjected to thousands or millions of years of postshock annealing and/or weathering. A useful intermediate case is that of nuclear detonation. Stress pulses for these events can reach 0.1 ms or higher, and samples are obtained in pristine condition. All three types of loading produce stresses of hundreds of kilobars. Samples studied were taken from the Sedan nulcear test site, and consist of a coarse-grained granodiorite containing quartz, K-feldspar, cordierite, and hornblende. Samples were studied optically in this section, then were thinned with an ion mill and studied by transmission electron microscopy (TEM). Optically, quartz and K-feldspar displayed numerous sets of planar deformation features (PDF's) identical to the nondecorated PDF's seen in laboratory samples and many natural impactites. TEM study showed that the PDF's in quartz and feldspar corresponded to densely packed wide transformation lamellae identical to those described in laboratory studies. The transformation lamellae in both minerals were amorphous, with no sign of high-pressure phases. In the case of K-feldspar only, narrow sublamellae extended outward from some wide lamellae. Quartz, which was more abundant and studied more extensively, contained no shock-induced dislocations. Some planar features were also seen in cordierite, but could not be identified due to rapid beam damage. No shock defects were seen in hornblende in TEM. The shock-induced defects present at the Sedan site are very similar to those seen in shock recovery experiments, and also to those present at certain natural events (e.g., Meteor Crater). This suggests that shock deformation in quartz is not strongly dependent on shock pulse duration, and that laboratory recovery experiments are useful simulations of natural impact events.

Gratz, A. J.↗

NASA NTRS1999

Delamination Modeling of Composites for Improved Crash Analysis

Finite element crash modeling of composite structures is limited by the inability of current commercial crash codes to accurately model delamination growth. Efforts are made to implement and assess delamination modeling techniques using a current finite element crash code, MSC/DYTRAN. Three methods are evaluated, including a straightforward method based on monitoring forces in elements or constraints representing an interface; a cohesive fracture model proposed in the literature; and the virtual crack closure technique commonly used in fracture mechanics. Results are compared with dynamic double cantilever beam test data from the literature. Examples show that it is possible to accurately model delamination propagation in this case. However, the computational demands required for accurate solution are great and reliable property data may not be available to support general crash modeling efforts. Additional examples are modeled including an impact-loaded beam, damage initiation in laminated crushing specimens, and a scaled aircraft subfloor structures in which composite sandwich structures are used as energy-absorbing elements. These examples illustrate some of the difficulties in modeling delamination as part of a finite element crash analysis.

Fleming, David C.↗

NASA NTRS1999

Delamination Modeling of Composites for Improved Crash Analysis

Fleming, David C.↗

NASA NTRS2013

Stardust Interstellar Preliminary Examination III: Infrared Spectroscopic Analysis of Interstellar Dust Candidates

Under the auspices of the Stardust Interstellar Preliminary Examination, picokeystones extracted from the Stardust Interstellar Dust Collector were examined with synchrotron Fourier transform infrared (FTIR) microscopy to establish whether they contained extraterrestrial organic material. The picokeystones were found to be contaminated with varying concentrations and speciation of organics in the native aerogel, which hindered the search for organics in the interstellar dust candidates. Furthermore, examination of the picokeystones prior to and post X-ray microprobe analyses yielded evidence of beam damage in the form of organic deposition or modification, particularly with hard X-ray synchrotron X-ray fluorescence. From these results, it is clear that considerable care must be taken to interpret any organics that might be in interstellar dust particles. For the interstellar candidates examined thus far, however, there is no clear evidence of extraterrestrial organics associated with the track and/or terminal particles. However, we detected organic matter associated with the terminal particle in Track 37, likely a secondary impact from the Al-deck of the sample return capsule, demonstrating the ability of synchrotron FTIR to detect organic matter in small particles within picokeystones from the Stardust interstellar dust collector.

Interstellar↗

NASA NTRS1998

Potential for EMU Fabric Damage by Electron Beam and Molten Metal During Space Welding for the International Space Welding Experiment

As a consequence of preparations concerning the International Space Welding Experiment (ISWE), studies were performed to better understand the effect of molten metal contact and electron beam impingement with various fabrics for space suit applications. The question arose as to what would occur if the electron beam from the Ukrainian Universal Hand Tool (UHT) designed for welding in space were to impinge upon a piece of Nextel AF-62 ceramic cloth designed to withstand temperatures up to 1427 C. The expectation was that the electron beam would lay down a static charge pattern with no damage to the ceramic fabric. The electron beam is capable of spraying the fabric with enough negative charge to repel further electrons from the fabric before significant heating occurs. The static charge pattern would deflect any further charge accumulation except for a small initial amount of leakage to the grounded surface of the welder. However, when studies were made of the effect of the electron beam on the insulating ceramic fabric it was surprisingly found that the electron beam did indeed burn through the ceramic fabric. It was also found that the shorter electron beam standoff distances had longer burnthrough times than did some greater electron beam standoff distances. A possible explanation for the longer burnthrough times for the small electron beam standoff distance would be outgassing of the fabric which caused the electron beam hand-tool to cycle on and off to provide some protection for the cathodes. The electron beam hand tool was observed to cycle off at the short standoff distance of two inches likely due to vapors being outgassed. During the electron beam welding process there is an electron leakage, or current leakage, flow from the fabric. A static charge pattern is initially laid down by the electron beam current flow. The static charge makes up the current leakage flow which initially slightly heats up the fabric. The initially laid down surface charge leaks a small amount of current. The rate at which the current charge leaks from the fabric controls how fast the fabric heats up. As the ceramic fabric is heated it begins to outgass primarily from contamination/impurities atoms or molecules on and below the fabric surface. The contaminant gases ionize to create extra charge carriers and multiply a current of electrons. The emitted gas which ionized in the electron leakage flow promotes further leakage. Thus, the small leakage of charge from the fabric surface is enhanced by outgassing. When the electron beam current makes up the lost current, the incoming electrons heat the fabric and further enhance the outgassing. The additional leakage promotes additional heating up of the ceramic fabric. The electrons bound to the ceramic fabric surface leak off more and more as the surface gets hotter promoting even greater leakage. The additional electrons that result also gain energy in the field and produce further electrons. Eventually the process becomes unstable and accelerates to the point where a hole is burned through the fabric.

Fragomeni, James M.↗

NASA NTRS1993

Compression of laminated composite beams with initial damage

The effect of isolated damage modes on the compressive strength and failure characteristics of laminated composite test specimens were evaluated experimentally and numerically. In addition to specimens without initial damage, specimens with three types of initial damage were considered: (1) specimens with short delaminations distributed evenly through the specimen thickness, (2) specimens with few long delaminations, and (3) specimens with local fiber damage in the surface plies under the three-point bend contact point. It was found that specimens with short multiple delamination experienced the greatest reduction in compression strength compared to the undamaged specimens. Single delaminations far from the specimen surface had little effect on the final compression strength, and moderate strength reduction was observed for specimens with localized surface ply damage.

Breivik, Nicole L.↗