Focused Ion Beam-Prepared Transmission Electron Microscopy Examination of Atmospheric Chemical Vapor-Infiltrated Silicon Carbide Morphology
Explore the source record for details and available documents.
Zachary Tobin↗
SEARCH · Search NASA
Results for “Focused Ion Beam”
Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.
Quote a phrase for an exact phrase match. Source license links do not imply unrestricted reuse.
Spherical ion source
Radial focusing of electrons in ion source produces greater ion densities, resulting in higher resolution and focus capability for a given source volume. Electron beam is focused near exit aperture by spherical fields. High density ions allow focusing ion beam to high density at echo, allowing high current through small aperture.
Hall, L. G.↗
13-kV Ion-Extraction System Being Developed for Inert Gas Ion Engines
A high-voltage ion optics design was chosen for an assumed outer planet or interstellar precursor mission that would require a long-life, high-power, high-specific-impulse krypton ion engine. Such an engine could support energetic space missions to the outer planets or beyond. Detailed performance and lifetime analyses and several inexpensive subscale grid tests were conducted at the NASA Glenn Research Center and at the Colorado State University under a NASA Glenn grant. A subscale grid set of the selected geometry shown was tested at voltages up to 13,000 V. This yielded a krypton ion beam current that would, when scaled to a full-size 50-cm diameter, produce an ion beam with a power of 30 kW at a specific impulse over 14,000 sec. The operational ion beam focusing limits, as a function of ion current per hole, were found to impose requirements of high uniformity on the discharge chamber plasma density. A full-size set of two-grid, 50-cm-diameter titanium ion optics has been fabricated and awaits testing.
Rawlin, Vincent K.↗
Some Aspects on the Mechanical Analysis of Micro-Shutters
An array of individually addressable micro-shutters is being designed for spectroscopic applications. Details of the design are presented in a companion paper. The mechanical design of a single shutter element has been completed. This design consists of a shutter blade suspended on a torsion beam manufactured out of single crystal silicon membranes. During operation the shutter blade will be rotated by 90 degrees out of the array plane. Thus, the stability and durability of the beams are crucial for the reliability of the devices. Structures were fabricated using focused ion beam milling in a FEI 620 dual beam machine, and subsequent testing was completed using the same platform. This allowed for short turn around times. We performed torsion and bending experiments to determine key characteristics of the membrane material. Results of measurements on prototype shutters were compared with the predictions of the numerical models. The data from these focused studies were used in conjunction with experiments and numerical models of shutter prototypes to optimize the design. In this work, we present the results of the material studies, and assess the mechanical performance of the resulting design.
Fettig, Rainer K.↗
Nuclear Microprobe using Elastic Recoil Detection (ERD) for Hydrogen Profiling in High Temperature Protonic Conductors
The interaction between hydrogen and various high temperature protonic conductors (HTPC) has not been clearly understood due to poor densification and unreacted secondary phases. the melt-processing technique is used in producing fully dense simple SrCe(0.9)Y (0.10) O(3-delta) and complex Sr3Ca(1+x)Nb(2+x)O(9-delta) perovskites that can not be achieved by solid-state sintering. the possibilities of ion beam analysis have been investigated to quantify hydrogen distribution in HTPC perovskites subjected to water heat treatment. Nuclear microprobe technique is based on the interactions of a focused ion beam of MeV light ions (H-1, H-2, He-3, He-4,.) with the sample to be analyzed to determine local elemental concentrations at the cubic micrometer scale, the elastic recoil detection analysis technique (ERDA) has been carried out using He-4(+) microbeams and detecting the resulting recoil protons. Mappings of longitudinal sections of water treated SrCeO3 and Sr(Ca(1/3)Nb(2/3))O3 perovskites have been achieved, the water treatment strongly alters the surface of simple SrCe(0.9)Y(0.10)O(3-delta) perovskite. From Rutherford Back Scattering measurements (RBS), both Ce depletion and surface re-deposition is evidenced. the ERDA investigations on water treated Sr3Ca(1+x)Nb(2+x)O(9-delta) perovskite did not exhibit any spatial difference for the hydrogen incorporation from the surface to the centre. the amount of hydrogen incorporation for Sr3Ca(1+x)Nb(2+x)O(9-delta) was low and required further development of two less conventional techniques, ERDA in forward geometry and forward elastic diffusion H-1(p,p) H-1 with coincidence detection.
Berger, Pascal↗
A Novel Hybrid Ultramicrotomy/FIB-SEM Technique: Preparation of Serial Electron-Transparent Thin Sections of a Hayabusa Grain
The Japanese space agency's (JAXA) Hayabusa mission returned the first particulate samples (typically <100micron) from the surface of an asteroid (25143 Itokawa). These precious samples provide important insights into early Solar System processes, but their sizes pose tremendous challenges to coordinated analysis using a variety of nano- and micro-beam techniques. The ability to glean maximal information from individual particles has become increasingly important and depends critically on sample preparation. We developed a hybrid technique combining traditional ultramicrotomy with focused ion beam (FIB) techniques, allowing for more thorough in situ investigations of grain surfaces and interiors. Using this method, we increase the number of FIB-prepared sections that can be recovered from a particle with dimensions on the order of tens of microns. These sections can be subsequently analyzed using a variety of analytical techniques. Particle RA-QD02-0211 is a approx. 40×40×20 micron particle from Itokawa containing olivine and Fe sulfides. It was embedded in low viscosity epoxy and partly sectioned to a depth of approx 10 micron; sections are placed on Cu grids with thin amorphous films for transmission electron microscope (TEM) analyses. With the sample surface partly exposed, the epoxy bullet is trimmed to a height of approx. 5mm to accommodate the allowable dimensions for FIB work (FEI Quanta 600 3D dual beam FIB-SEM). Using a diamond trim knife, the epoxy surrounding the grain is removed on 3 sides (to within a few microns of the grain); the depth of material removed extends well below the bottom of the particle. The sample is attached to an SEM pin mount, the epoxy coated with conductive paint, and the entire assembly coated with approx. 40nm of carbon to eliminate sample charging during FIB work. A protective carbon cap is placed according to the plan for the 15 FIB sections. The central 'spine' of the cap runs perpendicular to the front of the sample, and the 'ribs' protruding from either side run parallel. Each rib indicates the location of a planned FIB section, and the spine contains the final two planned sections. We use a cap with a 4 micron-wide spine and 2micron-wide ribs that have ≳3.5 micron of space between them (narrower cuts result in too much re-deposition of material inside the trenches). Using a 30kV, 3nA ion-beam we expose the front surface of the grain and commence milling trenches between sections. Rather than using the typical C-cut to prepare the sample for lift-out, an L-cut is used instead, leaving the sample connected by an interior tab. tab. Sections are lifted out, attached to TEM grids and thinned to electron transparency. TEM analyses show that our hybrid technique preserves both interior and edge features, including surface modifications from exposure to the space environment, such as damaged rims that form in response to solar wind implantation effects and adhering grains. In addition, the FIB sections provide larger areas that are free of fractures and chatter effects in comparison to the microtome thin sections, thus enabling more accurate measurements of solar flare particle track densities that are used to determine the surface exposure age of the particles.
Berger, Eve L.↗
Nanoscale Compositional Relations in Lunar Rock Patina: Deciphering Sources for Patina Components on an Apollo 17 Station 6 Boulder
Space weathering on the Moon and other airless bodies modifies the surfaces of regolith grains as well as the space-exposed surfaces of larger rocks and boulders. As space weathering witness plates, rocks and boulders are distinguished from regolith grains based on their ability to persist as physically intact substrates over longer time scales before being disaggregated by impact processes. Because lunar surfaces, including exposed rocks, quickly develop an optically thick layer of patina, it is important to understand the compositional relationship between patinas and their underlying rock substrates, particularly to support remote-sensing of rocky lunar terrains. Based on analytical TEM techniques, supported by focused ion beam (FIB) cross-sectioning, we have begun to systematize the multi-layer microstructural complexity of patinas on rock samples with a range of space exposure histories. Our on-going work has particularly focused on lunar rock 76015, both because it has a long (approx. 22 my) exposure history, and because its surface was exposed to patina development approximately 1 m off the regolith surface on a boulder in the Apollo 17 Station 6 boulder field. Potential sources for the 76015 patina therefore include impact-melted and vaporized material derived from the local rock substrate, as well as from the mix of large boulders and regolith in the Station 6 area. While similar, there are differences in the mineralogy and chemistry of the rocks and regolith at Station 6. We were interested to see if these, or other sources, could be distinguished in the average composition, as well as the compositional nanostratigraphy of the 76015 patina. To date we have acquired a total of 9 TEM FIB cross-sections from the 76015 patina, giving us reasonable confidence of being able to arrive at an integrated average for the patina major element composition based on analytical TEM methods.
Christoffersen, R.↗
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↗
Coordinated Microstructural and Isotopic Characterization of Diamond Inclusions within the Kenna Ureilite
Introduction: The origin of diamonds in ureilitic meteorites, a major family of ultramafic achondrites, has long been debated, with various formation mechanisms inferred, including: 1) shock conversion of preexisting graphite due to a hypervelocity impact on the ureilite parent body [e.g., 1]; 2) vapor deposition during condensation of the solar nebula [e.g., 2]; or 3) static transformation in the mantle of a large planetesimal (>1000 km in diameter) [e.g., 3]. The Kenna ureilite is a 10.9 kg stone that was found in Kansas in 1972 and is dominantly composed of olivine and pigeonite (68% and 22% modal abundance, respectively), together with minor metal and carbon-rich regions. Within the carbon-rich domains researchers have identified microdiamonds up to ~10 µm in size [4]. Methods: Due to the proximity of the extremely hard microdiamonds with soft graphite and moderately hard silicates, achieving an appropriately flat surface for electron backscatter diffraction (EBSD) analysis has proven challenging. We have, therefore, employed a Hitachi ArBlade 5000 broad beam Ar ion milling system to prepare a sample with an adequately uniform surface flatness across the various minerals. The ion milling dramatically im-proved indexing of the EBSD patterns and facilitated high-resolution microstructural analysis of the carbon-rich domains. After microstructural EBSD analyses using an Oxford Symmetry detector we collected coordinated hy-perspectral cathodoluminescence (CL) analyses using a Gatan Monarc system mounted on a JEOL 7900F field emission (FE) scanning electron microscope at NASA Johnson Space Center. A focused ion beam (FIB) foil was extracted from a region of interest and analyzed using a JEOL 2500 FE scanning transmission electron microscope (STEM). In situ carbon and nitrogen isotopic analyses were collected from diamond-bearing domains using a Cameca NanoSIMS 50L at NASA JSC. Results: The carbon rich regions occur as tabular domains between polygonal olivine and pigeonite, and are composed of aggregates of micrometer-scale diamond with intermediate graphite, oxides and metal grains. Within the microdiamonds, {111} twins are abundant, many of which form ragged lamellae consistent with mechanical twinning. The microdiamond assemblages appear to pseudomorph tabular graphite habits, which together with the abundant deformation twins, support a shock transformation mechanism for microdiamond formation within the Kenna meteorite. Further supporting this observation, the diamond laths show close alignment of <111> and <110> between domains, consistent with a solid-state transformation from graphite along <0001> and <1-210>, respec-tively [5]. A FIB foil was extracted from a region with mechanical twins, and high resolution STEM analyses reveal cross-cutting veins of graphite and oriented kamacite crystals together with additional sets of {111} nano-twins formed in at least three orientations. Isotopic analyses of C and N reveal sector zoning patterns [cf. 3] that are unre-lated to the diamond substructure identified by EBSD yet consistent with hyperspectral CL images. Conclusions: These data provide new constraints on microdiamond formation within ureilites. The microdia-monds exhibit orientation variants defined by aligned <111> and <110> axes consistent with inherited crystallo-graphic orientations from transformation of a single hexagonal graphite parent crystal [5]. Crosscutting the micro-diamonds are veins of graphite and kamacite, together with additional {111} nanotwins. Taken together these data suggest that microdiamonds from ureilites formed from a solid state, diffusionless transformation from graphite, likely associated with a major shock event, which was subject to subsequent reversion either during decompression or a later deformation event. The N and C isotopic sector zoning is unrelated to diamond microstructures and likely reflects inheritance from the parent graphite crystal.
Ureilite↗
Indigenous Carbonaceous Matter in the Nakhla Mars Meteorite
Detailed microanalysis of the Martian meteorite Nakhla has shown there are morphologically distinct carbonaceous features spatially associated with low-T aqueous alteration phases including salts and id-dingsite. A comprehensive suite of analytical instrumentation including optical microscopy, field emission scanning electron microscopy (FESEM), energy dispersive X-ray (EDX) spectroscopy, focused ion beam (FIB) microscopy, transmission electron microscopy (TEM), two-step laser mass spectrometry (mu-L(sup 2)MS), laser mu-Raman spectroscopy, Fourier transform infrared spectroscopy (FTIR), and nanoscale secondary ion mass spectrometry (NanoSIMS) are being used to characterize the carbonaceous matter and host mineralogy. The search for carbonaceous matter on Mars has proved challenging. Viking Landers failed to unambiguously detect simple organics at either of the two landing sites although the Martian surface is estimated to have acquired at least 10(exp15) kg of C as a consequence of meteoritic accretion over the last several Ga. The dearth of organics at the Martian surface has been attributed to various oxidative processes including UV photolysis and peroxide activity. Consequently, investigations of Martian organics need to be focused on the sub-surface regolith where such surface processes are either severely attenuated or absent. Fortuitously since Martian meteorites are derived from buried regolith materials they provide a unique opportunity to study Martian organic geochemistry.
Clemett, S. J.↗
Investigation of kilovolt ion sputtering second quarterly progress report
Kilovolt ion sputtering - electron beam focusing of cesium ion beam, radiation detection in copper atoms, ultrahigh vacuum system construction, and spectrometer pulse height
COPPER↗
Increased capabilities of the 30-cm diameter Hg ion thruster
A 30-cm-diam mercury ion thruster, using two or three grid ion accelerating systems, is operated at increased values of beam current. Comparisons with the SEP (Solar Electric Propulsion) and EPSEP (Extended Performance SEP) baseline thrusters are made with respect to performance and lifetime. It is found that when a third, or decelerator, grid is added to the conventional two-grid optics of a SEP-like thruster, the ion beam focusing properties are improved, as expected from theoretical considerations. The total thruster efficiency as a function of specific impulse, is increased for values of specific impulse in the range 1200-2800 sec. Lifetime test results predict a thruster lifetime, under space conditions, not less than that of the baseline SEP thruster.
Rawlin, V. K.↗
Durable High-Density Data Storage
The focus ion beam (FIB) micromilling process for data storage provides a new non-magnetic storage method for archiving large amounts of data. The process stores data on robust materials such as steel, silicon, and gold coated silicon. The storage process was developed to provide a method to insure the long term storage life of data. We estimate that the useful life of data written on silicon or gold-coated silicon to be on the order of a few thousand years without the need to rewrite the data every few years. The process uses an ion beam to carve material from the surface, much like stone cutters in ancient civilizations removed material from stone. The deeper the information is carved into the media, the longer the expected life of the information. The process can record information in three formats: (1) binary at densities of 23 Gbits/square inch, (2) alphanumeric at optical or non-optical density, and (3) graphical at optical and non-optical density. The formats can be mixed on the same media; and thus, it is possible to record, in a human-viewable format, instructions that can be read using an optical microscope. These instructions provide guidance on reading the remaining higher density information.
Lamartine, Bruce C.↗
Fracture Probability of MEMS Optical Devices for Space Flight Applications
A bending fracture test specimen design is presented for thin elements used in optical devices for space flight applications. The specimen design is insensitive to load position, avoids end effect complications, and can be used to measure strength of membranes less than 2 microns thick. The theoretical equations predicting stress at failure are presented, and a detailed finite element model is developed to validate the equations for this application. An experimental procedure using a focused ion beam machine is outlined, and results from preliminary tests of 1.9 microns thick single crystal silicon are presented. These tests are placed in the context of a methodology for the design and evaluation of mission critical devices comprised of large arrays of cells.
Fettig, Rainer K.↗
High Resolution Chemical Study of ALH84001
We have studied the chemistry of a sample of the SNC meteorite ALH84001 using an environmental scanning electron microscope (ESEM) with an energy dispersive chemical analytical detector and a focused ion beam secondary ion mass spectrometer (FIB-SIMS). Here we present the chemical data, both spectra and images, from two techniques that do not require sample preparation with a conductive coating, thus eliminating the possibility of preparation-induced textural artifacts. The FIB-SIMS instrument includes a column optimized for SEM with a quadrupole type mass spectrometer. Its spatial and spectral resolution are 20 nm and 0.4 AMU, respectively. The spatial resolution of the ESEM for chemical analysis is about 100 nm. Limits of detection for both instruments are mass dependent. Both the ESEM and the FIB-SIMS instrument revealed contrasting surficial features; crumbled, weathered appearance of the matrix in some regions as well as a rather ubiquitous presence of euhedral halite crystals, often associated with cracks or holes in the surface of the rock. Other halogen elements present in the vicinity of the NaCl crystals include K and Br. In this report, elemental inventories are shown as mass spectra and as X-ray maps.
Conrad, Pamela G.↗
Transmission Electron Microscopy of an In Situ Presolar Silicon Carbide Grain
We used a focused ion beam workstation to prepare ultra-thin sections of a presolar SiC grain. Our TEM studies indicate that the SiC formed by rapid vapor-phase condensation, trapping pre-existing graphite grains in random orientations. Additional information is contained in the original extended abstract.
Stroud, Rhonda M.↗
Lunar and Planetary Science XXXV: Interplanetary Dust and Aerogel
Contents include the following: Isotopically Primitive Interplanetary Dust Particles of Cometary Origin: Evidence from Nitrogen Isotopic Compositions. The Solar Nebula s First Accretionary Particles (FAPs) Are They Preserved in Collected Interplanetary Dust Samples? On the Origin of GEMS. An Analytical SuperSTEM for Extraterrestrial Materials Research. Sub-Micrometer Scale Minor Element Mapping in Interplanetary Dust Particles: A Test for Stratospheric Contamination. First Report of Taenite in an Asteroidal Interplanetary Dust Particle: Flash-heating Simulates Nebular Dust Evolution. FTIR Analyses of IDPs: Comparison with the InfraRed Spectra of the Interstellar Medium. Mineralogical Study of Hydrated IDPs: X-Ray Diffraction and Transmission Electron Microscopy. Focused Ion Beam Recovery and Analysis of Interplanetary Dust Particles (IDPs) and Stardust Analogues. Technique for Concentration of Carbonaceous Material from Aerogel Collectors Using HF-Vapor Etching. Synchrotron X-Ray Analysis of Captured Particle Residue in Aerogel. In-Situ Analyses of Earth Orbital Grains Trapped in Aerogel, Using Synchrotron X-Ray Microfluorescence Techniques. Igneous Rims on Micrometeorites and the Sizes of Chondrules in Main Belt Asteroids.
Source record↗