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At least 109 records · Page 6
All sourcesNASA NTRSDOE OSTI
DOE OSTI2023

Reflective Fiber Temperature Probe Based on Localized Surface Plasmon Resonance towards Low-Cost and Wireless Interrogation

Reflection fiber temperature sensors functionalized with plasmonic nanocomposite material using intensity-based modulation are demonstrated for the first time. Characteristic temperature optical response of the reflective fiber sensor is experimentally tested using Au-incorporated nanocomposite thin films deposited on the fiber tip, and theoretically validated using a thin-film-optic-based optical waveguide model. By optimizing the Au concentration in a dielectric matrix, Au nanoparticles (NP) exhibit a localized surface plasmon resonance (LSPR) absorption band in a visible wavelength that shows a temperature sensitivity ~0.025%/°C as a result of electron–electron and electron–phonon scattering of Au NP and the surrounding matrix. Detailed optical material properties of the on-fiber sensor film are characterized using scanning electron microscopy (SEM) and focused-ion beam (FIB)-assisted transmission electron microscopy (TEM). Airy’s expression of transmission and reflection using complex optical constants of layered media is used to model the reflective optical waveguide. A low-cost wireless interrogator based on a photodiode transimpedance-amplifier (TIA) circuit with a low-pass filter is designed to integrate with the sensor. The converted analog voltage is wirelessly transmitted via 2.4 GHz Serial Peripheral Interface (SPI) protocols. Feasibility is demonstrated for portable, remotely interrogated next-generation fiber optic temperature sensors with future capability for monitoring additional parameters of interest.

47 OTHER INSTRUMENTATION↗
DOE OSTI2024

Focused Ion Beam Tomography of Alloy 617 Corroded in Molten Chloride Salt

Materials qualification of reactor structural materials is a critical step in rapid implementation of advanced nuclear reactor technologies, particularly to assess the corrosion performance in these designs. Accelerated qualification of reactor structural materials requires incorporating powerful computational toolsets, such as phase field modelling in the Multiphysics Object-Oriented Simulation Environment (MOOSE) framework, to predict the evolution of structural materials due to corrosion. Accordingly, computational toolsets will require experimental data generated at appropriate length scales to validate accuracy. Focused ion beam (FIB) provides a high degree of control over manipulation of materials for analytical purposes, including capturing data on the evolution in the microstructure and elemental composition of materials at the mesoscale, an appropriate length scale for phase field modelling of intergranular diffusion phenomena using the MOOSE framework. For instance, the FEI Helios G4 UX dual beam plasma FIB microscope at the Irradiated Materials Characterization Laboratory (IMCL) is capable of backscatter diffraction (EBSD) and energy-dispersive x-ray spectroscopy (EDS) documenting the evolution in the microstructure and elemental composition, respectively. The Helios can perform EDS and EBSD three-dimensionally (3D) using tomography, which is then combined using different software packages to visualize 3D volumes correlating elemental composition to microstructural data. The purpose of this investigation was to develop a streamlined characterization and data processing workflow for 3D tomography studies on the FEI Helios G4 plasma FIB. The investigation is segmented into three parts: 1) Optimizing the data collection workflow, 2) identifying appropriate data processing and visualization software (i.e. DREAM.3D, MIPAR, and VGStudioMax), and 3) establishing an infrastructure for public release. The optimization of the data collection workflow is in collaboration with members of the U220 department to setup formal training on the tomography operation of the G4, through ThermoFisher Scientific, and exploring DREAM.3D, MIPAR, and VGStudioMax data processing/visualization software packages. VGStudioMax currently demonstrates the most promise for future use. Optimization of the data collection and processing workflow is still ongoing. A collaboration with INL High Performance Computing (HPC) established an open-source license for expediting the public release of FIB tomography datasets through HPC. FIB tomography data generated by the G4 will provide comprehensive data for validating 3D phase field mesoscale modelling tools within the MOOSE framework for accelerated qualification of reactor structural materials.

Copeland-Johnson, Trishelle↗
NASA NTRS1996

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.↗
NASA NTRS2004

Focused Ion Beam Recovery and Analysis of Interplanetary Dust Particles (IDPs) and Stardust Analogues

Meteoritics research is a major beneficiary of recent developments in analytical instrumentation [1,2]. Integrated studies in which multiple analytical techniques are applied to the same specimen are providing new insight about the nature of IDPs [1]. Such studies are dependent on the ability to prepare specimens that can be analyzed in multiple instruments. Focused ion beam (FIB) microscopy has revolutionized specimen preparation in materials science [3]. Although FIB has successfully been used for a few IDP and meteorite studies [1,4-6], it has yet to be widely utilized in meteoritics. We are using FIB for integrated TEM/NanoSIMS/synchrotron infrared (IR) studies [1].

Graham, G. A.↗
NASA NTRS2005

Focused Ion Beam Microscopy of ALH84001 Carbonate Disks

Our aim is to understand the mechanism(s) of formation of carbonate assemblages in ALH84001. A prerequisite is that a detailed characterization of the chemical and physical properties of the carbonate be established. We present here analyses by transmission electron microscopy (TEM) of carbonate thin sections produced by both focused ion beam (FIB) sectioning and ultramicrotomy. Our results suggest that the formation of ALH84001 carbonate assemblages were produced by considerably more complex process(es) than simple aqueous precipitation followed by partial thermal decomposition as proposed by other investigators [e.g., 1-3].

Thomas-Keprta, Kathie L.↗
NASA NTRS2001

Fast prototyping of high-aspect ratio, high-resolution x-ray masks by gas-assisted focused ion beam

The capacity of chemically-assisted focused ion beam (fib) etching systems to undertake direct and highly anisotropic erosion of thin and thick gold (or other high atomic number [Z])coatings on x-ray mask membranes/substrates provides new levels of precision, flexibility, simplification and rapidity in the manufacture of mask absorber patterns, allowing the fast prototyping of high aspect ratio, high-resolution masks for deep x-ray lithography.

fast prototyping of high-aspect ratio high-resolut↗
NASA NTRS2007

Probing the Depths of Space Weathering: A Cross-sectional View of Lunar Rock 76015

The term "space weathering" refers to the cumulative effects of several processes operating at the surface of any solar system body not protected by a thick atmosphere. These processes include cosmic and solar ray irradiation, solar wind implantation and sputtering, as well as melting and vaporization due to micrometeorite bombardment. Space weathering discussions have generally centered around soils but exposed rocks will also incur the effects of weathering. Rocks have much longer surface lifetimes than an individual soil grain and thus record a longer history of exposure. By studying the weathering products which have built up on a rock surface, we can gain a deeper perspective on the weathering process and better assess the relative importance of various weathering components. The weathered coating, or patina, of the lunar rock 76015 has been previously studied using SEM and TEM. It is a noritic breccia with both "glazed" (smooth glassy) and "classic" (microcratered and pancake-bearing) patina coatings. Previous TEM work on 76015 relied on ultramicrotomy to prepare cross sections of the patina coating, but these sections were limited by the "chatter" and loss of material in these brittle samples. Here we have used a focused ion beam (FIB) instrument to prepare cross sections in which the delicate stratigraphy of the patina coating is beautifully preserved.

Noble, Sarah K.↗
NASA NTRS2008

Transmission Electron Microscopy of Cometary Residues from Micron-Sized Craters in the Stardust Al-Foils

We report Transmission Electron Microscopy (TEM) investigations of micro-craters that originated from hypervelocity impacts of comet 81P/Wild 2 dust particles on the aluminium foil of the Stardust collector. The craters were selected by Scanning Electron Microscopy (SEM) and then prepared by Focused Ion Beam (FIB) milling techniques in order to provide electron transparent cross-sections for TEM studies. The crater residues contain both amorphous and crystalline materials in varying proportions and compositions. The amorphous component is interpreted as resulting from shock melting during the impact and the crystalline phases as relict minerals. The latter show evidence for shock metamorphism. Based on the residue morphology and the compositional variation, the impacting particles are inferred to have been dominated by mixtures of submicron olivine, pyroxene and Fe-sulfide grains, in agreement with prior results of relatively coarse-grained mineral assemblages in the aerogel collector.

Leroux, Hugues↗
NASA NTRS2006

Microstructural Study of Micron-Sized Craters Simulating Stardust Impacts in Aluminum 1100 Targets

Various microscopic techniques were used to characterize experimental micro- craters in aluminium foils to prepare for the comprehensive analysis of the cometary and interstellar particle impacts in aluminium foils to be returned by the Stardust mission. First, SEM (Scanning Electron Microscopy) and EDS (Energy Dispersive X-ray Spectroscopy) were used to study the morphology of the impact craters and the bulk composition of the residues left by soda-lime glass impactors. A more detailed structural and compositional study of impactor remnants was then performed using TEM (Transmission Electron Microscopy), EDS, and electron diffraction methods. The TEM samples were prepared by Focused Ion Beam (FIB) methods. This technique proved to be especially valuable in studying impact crater residues and impact crater morphology. Finally, we also showed that InfraRed microscopy (IR) can be a quick and reliable tool for such investigations. The combination of all of these tools enables a complete microscopic characterization of the craters.

Leroux, Hugues↗
NASA NTRS2006

Focused Ion Beam Recovery of Hypervelocity Impact Residue in Experimental Craters on Metallic Foils

The Stardust sample return capsule will return to Earth in January 2006 with primitive debris collected from Comet 81P/Wild-2 during the fly-by encounter in 2004. In addition to the cometary particles embedded in low-density silica aerogel, there will be microcraters preserved in the Al foils (1100 series; 100 micrometers thick) that are wrapped around the sample tray assembly. Soda lime spheres (approximately 49 m in diameter) have been accelerated with a light-gas-gun into flight-grade Al foils at 6.35 km s(sup -1) to simulate the potential capture of cometary debris. The preserved crater penetrations have been analyzed using scanning electron microscopy (SEM) and x-ray energy dispersive spectroscopy (EDX) to locate and characterize remnants of the projectile material remaining within the craters. In addition, ion beam induced secondary electron imaging has proven particularly useful in identifying areas within the craters that contain residue material. Finally, high-precision focused ion beam (FIB) milling has been used to isolate and then extract an individual melt residue droplet from the interior wall of an impact penetration. This enabled further detailed elemental characterization, free from the background contamination of the Al foil substrate. The ability to recover pure melt residues using FIB will significantly extend the interpretations of the residue chemistry preserved in the Al foils returned by Stardust.

Graham, G. A.↗
NASA NTRS2003

New Methods of Sample Preparation for Atom Probe Specimens

Magnetite is a common conductive mineral found on Earth and Mars. Disk-shaped precipitates approximately 40 nm in diameter have been shown to have manganese and aluminum concentrations. Atom-probe field-ion microscopy (APFIM) is the only technique that can potentially quantify the composition of these precipitates. APFIM will be used to characterize geological and planetary materials, analyze samples of interest for geomicrobiology; and, for the metrology of nanoscale instrumentation. Prior to APFIM sample preparation was conducted by electropolishing, the method of sharp shards (MSS), or Bosch process (deep reactive ion etching) with focused ion beam (FIB) milling as a final step. However, new methods are required for difficult samples. Many materials are not easily fabricated using electropolishing, MSS, or the Bosch process, FIB milling is slow and expensive, and wet chemistry and the reactive ion etching are typically limited to Si and other semiconductors. APFIM sample preparation using the dicing saw is commonly used to section semiconductor wafers into individual devices following manufacture. The dicing saw is a time-effective method for preparing high aspect ratio posts of poorly conducting materials. Femtosecond laser micromachining is also suitable for preparation of posts. FIB time required is reduced by about a factor of 10 and multi-tip specimens can easily be fabricated using the dicing saw.

rock varnish↗
NASA NTRS2007

Fabrication of Buried Nanochannels From Nanowire Patterns

A method of fabricating channels having widths of tens of nanometers in silicon substrates and burying the channels under overlying layers of dielectric materials has been demonstrated. With further refinement, the method might be useful for fabricating nanochannels for manipulation and analysis of large biomolecules at single-molecule resolution. Unlike in prior methods, burying the channels does not involve bonding of flat wafers to the silicon substrates to cover exposed channels in the substrates. Instead, the formation and burying of the channels are accomplished in a more sophisticated process that is less vulnerable to defects in the substrates and less likely to result in clogging of, or leakage from, the channels. In this method, the first step is to establish the channel pattern by forming an array of sacrificial metal nanowires on an SiO2-on-Si substrate. In particular, the wire pattern is made by use of focused-ion-beam (FIB) lithography and a subsequent metallization/lift-off process. The pattern of metal nanowires is then transferred onto the SiO2 layer by reactive-ion etching, which yields sacrificial SiO2 nanowires covered by metal. After removal of the metal covering the SiO2 nanowires, what remains are SiO2 nanowires on an Si substrate. Plasma-enhanced chemical vapor deposition (PECVD) is used to form a layer of a dielectric material over the Si substrate and over the SiO2 wires on the surface of the substrate. FIB milling is then performed to form trenches at both ends of each SiO2 wire. The trenches serve as openings for the entry of chemicals that etch SiO2 much faster than they etch Si. Provided that the nanowires are not so long that the diffusion of the etching chemicals is blocked, the sacrificial SiO2 nanowires become etched out from between the dielectric material and the Si substrate, leaving buried channels. At the time of reporting the information for this article, channels 3 m long, 20 nm deep, and 80 nm wide (see figure) had been fabricated by this method.

Choi, Daniel↗
NASA NTRS2010

Metal/Silicate Partitioning at High Pressures and Temperatures

The behavior of siderophile elements during metal-silicate segregation, and their resulting distributions provide insight into core formation processes. Determination of partition coefficients allows the calculation of element distributions that can be compared to established values of element abundances in the silicate (mantle) and metallic (core) portions of the Earth. Moderately siderophile elements, including W, are particularly useful in constraining core formation conditions because they are sensitive to variations in T, P, oxygen fugacity (fO2), and silicate composition. To constrain the effect of pressure on W metal/silicate partitioning, we performed experiments at high pressures and temperatures using a multi anvil press (MAP) at NASA Johnson Space Center and laser-heated diamond anvil cells (LHDAC) at the University of Maryland. Starting materials consisted of natural peridotite mixed with Fe and W metals. Pressure conditions in the MAP experiments ranged from 10 to 16 GPa at 2400 K. Pressures in the LHDAC experiments ranged from 26 to 58 GPa, and peak temperatures ranged up to 5000 K. LHDAC experimental run products were sectioned by focused ion beam (FIB) at NASA JSC. Run products were analyzed by electron microprobe using wavelength dispersive spectroscopy. Liquid metal/liquid silicate partition coefficients for W were calculated from element abundances determined by microprobe analyses, and corrected to a common fO2 condition of IW-2 assuming +4 valence for W. Within analytical uncertainties, W partitioning shows a flat trend with increasing pressure from 10 to 16 GPa. At higher pressures, W becomes more siderophile, with an increase in partition coefficient of approximately 0.5 log units.

Shofner, G.↗
NASA NTRS2010

Estimating the Probability of Electrical Short Circuits from Tin Whiskers

To comply with lead-free legislation, many manufacturers have converted from tin-lead to pure tin finishes of electronic components. However, pure tin finishes have a greater propensity to grow tin whiskers than tin-lead finishes. Since tin whiskers present an electrical short circuit hazard in electronic components, simulations have been developed to quantify the risk of said short circuits occurring. Existing risk simulations make the assumption that when a free tin whisker has bridged two adjacent exposed electrical conductors, the result is an electrical short circuit. This conservative assumption is made because shorting is a random event that had an unknown probability associated with it. Note however that due to contact resistance electrical shorts may not occur at lower voltage levels. In our first article we developed an empirical probability model for tin whisker shorting. In this paper, we develop a more comprehensive empirical model using a refined experiment with a larger sample size, in which we studied the effect of varying voltage on the breakdown of the contact resistance which leads to a short circuit. From the resulting data we estimated the probability distribution of an electrical short, as a function of voltage. In addition, the unexpected polycrystalline structure seen in the focused ion beam (FIB) cross section in the first experiment was confirmed in this experiment using transmission electron microscopy (TEM). The FIB was also used to cross section two card guides to facilitate the measurement of the grain size of each card guide's tin plating to determine its finish .

Courey, Karim J.↗
NASA NTRS2011

FE and MG Isotopic Analyses of Isotopically Unusual Presolar Silicate Grains

Interstellar and circumstellar silicate grains are thought to be Mg-rich and Fe-poor, based on astronomical observations and equilibrium condensation models of silicate dust formation in stellar outflows. On the other hand, presolar silicates isolated from meteorites have surprisingly high Fe contents and few Mg-rich grains are observed. The high Fe contents in meteoritic presolar silicates may indicate they formed by a non-equilibrium condensation process. Alternatively, the Fe in the stardust grains could have been acquired during parent body alteration. The origin of Fe in presolar silicates may be deduced from its isotopic composition. Thus far, Fe isotopic measurements of presolar silicates are limited to the Fe-54/Fe-56 ratios of 14 grains. Only two slight anomalies (albeit solar within error) were observed. However, these measurements suffered from contamination of Fe from the adjacent meteorite matrix, which diluted any isotopic anomalies. We have isolated four presolar silicates having unusual O isotopic compositions by focused ion beam (FIB) milling and obtained their undiluted Mg and Fe isotopic compositions. These compositions help to identify the grains stellar sources and to determine the source of Fe in the grains.

Nguyen, A. N.↗
NASA NTRS2011

Nakhla: a Martian Meteorite with Indigenous Organic Carbonaceous Features

The Nakhla meteorite possesses discrete, well defined, structurally coherent morphologies of carbonaceous phases present within iddingsite alteration zones. Based upon both isotopic measurements and analysis of organic phases the presence of pre-terrestrial organics is now recognized. Within the microcrystalline layers of Nakhla s iddingsite, discrete clusters of salt crystals are present. These salts are predominantly halite (NaCl) with minor MgCl2 crystals. Some CaSO4, likely gypsum, appears to be partially intergrown with some of the halite. EDX mapping shows discrete C-rich features are interspersed among these crystals. A hollow semi-spherical bowl structure (~ 3 m ) has been identified and analyzed after using a focused ion beam (FIB) to cut a transverse TEM thin section of the feature and the underlying iddingsite. TEM/EDX analysis reveals that the feature is primarily carbonaceous containing C with lesser amounts of Si, S, Ca, Cl, F, Na, and minor Mn and Fe; additionally a small peak consistent with N, which has been previously seen in Nakhla carbonaceous matter, is also present. Selected area electron diffraction (SAED) shows that this C-rich material is amorphous (lacking any long-range crystallographic order) and is not graphite or carbonate. Micro-Raman spectra acquired from the same surface from which the FIB section was extracted demonstrate a typical kerogen-like D and G band structure with a weak absorption peak at 1350 and a stronger peak at 1600/cm. The C-rich feature is intimately associated with both the surrounding halite and underlying iddingsite matrix. Both iddingsite and salts are interpreted as having formed as evaporate assemblages from progressive evaporation of water bodies on Mars. This assemblage, sans the carbonaceous moieties, closely resembles iddingsite alteration features previously described which were interpreted as indigenous Martian assemblages. These distinctive macromolecular carbonaceous structures in Nakhla may represent one of the sources of the high molecular weight organic material previously identified in Nakhla. While we do not speculate on the origin of these unique carbonaceous structures, we note that the significance of such observations is that it may allow us to construct a C-cycle for Mars based on the C chemistry of the Martian meteorites with obvious implications for astrobiology and the prebiotic evolution of Mars. In any case, our observations strongly suggest that organic C exists as micrometersize, discrete structures on Mars.

McKay, D. S.↗
NASA NTRS2011

An Examination of the Space Weathering Patina of Lunar Rock 76015

Space weathering discussions have generally centered around soils but exposed rocks will also incur the effects of weathering. Rocks have much longer surface lifetimes than an individual soil grain and thus record a longer history of exposure. By studying the weathering products which have built up on a rock surface, we can gain a deeper perspective on the weathering process and better assess the relative importance of various weathering components. The weathered coating, or patina, of the lunar rock 76015 has been previously studied under SEM and also by TEM using ultramicrotome sample preparation methods. However, to really understand the products involved in creating these coatings, it is helpful to examine the patina in cross section, something which is now possible though the use of Focused Ion Beam (FIB) sample prep techniques, which allows us to preserve intact the delicate stratigraphy of the patina coating and provides a unique cross-sectional view of the space weathering process. Several samples have been prepared from the rock and the coatings are found to be quite variable in thickness and composition from one sample to the next.

Noble, S.↗
NASA NTRS2008

An Investigation of the Electrical Short Circuit Characteristics of Tin Whiskers

Existing risk simulations make the assumption that when a free tin whisker has bridged two adjacent exposed electrical conductors, the result is an electrical short circuit. This conservative assumption is made because shorting is a random event that has a currently unknown probability associated with it. Due to contact resistance electrical shorts may not occur at lower voltage levels. In this experiment, we study the effect of varying voltage on the breakdown of the contact resistance which leads to a short circuit. From this data we can estimate the probability of an electrical short, as a function of voltage, given that a free tin whisker has bridged two adjacent exposed electrical conductors. Also, three tin whiskers grown from the same Space Shuttle Orbiter card guide used in the aforementioned experiment were cross-sectioned and studied using a focused ion beam (FIB). The rare polycrystalline structure seen in the FIB cross section was confirmed using transmission electron microscopy (TEM). The FIB was also used to cross section two card guides to facilitate the measurement of the grain size to determine that the tin plating on the card guides had a bright finish.

Courey, Karim J.↗