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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.

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At least 397 records · Page 22
All sourcesNASA NTRSDOE OSTI
NASA NTRS2001

AMINO ACID ANALYSES OF THE ANTARCTIC CM2 METEORITES ALH 83100 AND LEW 90500 USING LIQUID CHROMATOGRAPHY-TIME OF FLIGHT-MASS SPECTROMETRY

The investigation of organic compounds in primitive carbonaceous meteorites provides a record of the chemical processes that occurred in the early solar system. In particular, amino acids have been shown to be potential indicators in tracing the nature of carbonaceous chondrite parent bodies [ 13. The delivery of amino acids by carbonaceous chondrites to the early Earth could have been any important source of the Earth's prebiotic organic inventory [2]. Over 80 different amino acids have been detected in the Murchison CM2 meteorite, most of them completely non-existent in the terrestrial biosphere [3]. We have optimized a new liquid chromatography-time-of-flight-mass spectrometry (LC-ToF-MS) technique coupled with OPAMAC derivatization in order to detect amino acids in meteorite extracts by UV fluorescence and exact mass simultaneously. The detection limit of the LC-ToF-MS instrument for amino acids is at least 3 orders of magnitude lower than traditional GC-MS techniques. Here we report on the first analyses of amino acids and their enantiomeric abundances in the CM2 carbonaceous meteorites ALH 83100, LEW 90500, and Murchison using this new LC-ToF-MS instrument configuration. Amino acid analyses of any kind for the CM meteorite ALH 83100 have not previously been reported.

Glavin, D. P.↗
NASA NTRS2006

Composition of Pickup Ions at Titan Observed by the Cassini Plasma Spectrometer

Pickup ions have been observed in Saturn's rotating magnetosphere near Titan by the Cassini Plasma Spectrometer (CAPS) instrument during the Cassini orbiter's recent flybys of the moon. A preliminary analysis of the CAPS Time of Flight (TOF) spectra of the pickup ions observed during the TA flyby indicated the presence of H(+), H2(+), N(+)/CH2(+), CH4(+), and N2(+). These ions slow down Saturn's magnetospheric plasma beyond Titan's ionosphere through mass loading. Because of its relatively high mass and high concentration, CH4(+) is the dominant mass loading ion. The other ions make negligible contributions to the mass loading process except for N2(+) just above the ionopause, where its concentration becomes important. With the exception of CH2(+), the pickup ion sources are the neutral exosphere constituents H, H2, N, CH4, and N2, where CH2 is a fragment of the parents CH4 and CH4(+). A more detailed analysis of CAPS TOF spectra and empirical cracking patterns is carried out to determine the relative concentrations of N(+) and CH2(+). Although, the 28 amu ion was identified as N2(+), consistent with the dominance of its neutral source, N2, just above the ionopause, the ionospheric ion HCNH(+) may also be present. The possible leakage of this and other ionospheric ions such as CH5(+) into the pickup ion /mass loading region is also examined by further analysis of the corresponding TOF spectra.

Hartle, R.↗
NASA NTRS2006

Time of flight system on a chip

A CMOS time-of-flight TOF system-on-a-chip SoC for precise time interval measurement with low power consumption and high counting rate has been developed. The analog and digital TOF chip may include two Constant Fraction Discriminators CFDs and a Time-to-Digital Converter TDC. The CFDs can interface to start and stop anodes through two preamplifiers and perform signal processing for time walk compensation (110). The TDC digitizes the time difference with reference to an off-chip precise external clock (114). One TOF output is an 11-bit digital word and a valid event trigger output indicating a valid event on the 11-bit output bus (116).

Paschalidis, Nicholas P.↗
NASA NTRS2008

Simulation of a Miniature, Low-Power Time-of-Flight Mass Spectrometer for In Situ Analysis of Planetary Atmospheres

We are implementing nano- and micro-technologies to develop a miniaturized electron impact ionization mass spectrometer for planetary science. Microfabrication technology is used to fabricate the ion and electron optics, and a carbon nanotube (CNT) cathode is used to generate the ionizing electron beam. Future NASA planetary science missions demand miniaturized, low power mass spectrometers that exhibit high resolution and sensitivity to search for evidence of past and present habitability on the surface and in the atmosphere of priority targets such as Mars, Titan, Enceladus, Venus, Europa, and short-period comets. Toward this objective, we are developing a miniature, high resolution reflectron time-of-flight mass spectrometer (Mini TOF-MS) that features a low-power CNT field emission electron impact ionization source and microfabricated ion optics and reflectron mass analyzer in a parallel-plate geometry that is scalable. Charged particle electrodynamic modeling (SIMION 8.0.4) is employed to guide the iterative design of electron and ion optic components and to characterize the overall performance of the Mini TOF-MS device via simulation. Miniature (less than 1000 cubic centimeters) TOF-MS designs (ion source, mass analyzer, detector only) demonstrate simulated mass resolutions greater than 600 at sensitivity levels on the order of 10(exp -3) cps/molecule N2/cc while consuming 1.3 W of power and are comparable to current spaceflight mass spectrometers. Higher performance designs have also been simulated and indicate mass resolutions approximately 1000, though at the expense of sensitivity and instrument volume.

King, Todd T.↗
NASA NTRS2008

Miniature Mass Spectrometers on Space and Planetary Missions

Space flight mass spectrometers contribute our understanding of the origin and evolution of our solar system and even of life itself. This fundamental role has motivated increasing interest in miniature mass spectrometry for planetary missions. Several remarkable new instruments are en route or under development to investigate the composition of planetary bodies such as Mars and comets. For instance, the Sample Analysis at Mars (SAM) suite on the 2009 Mars Science Laboratory (MSL) mission includes a quadrupole mass spectrometer with a sophisticated gas processing system as well as pyrolysis and chemical derivatization protocols for solid samples. Future missions will require even lighter, lower power, and yet more capable mass spectrometers, particularly to analyze samples in situ on planetary surfaces. We have been developing laser-based mass spectrometers for elemental and organic/molecular analysis of rock, ice, or fine particle samples. These typically use time-of-flight (TOF) mass analyzers, which are readily miniaturized and can detect both atomic species and complex organics that occur in a variety of planetary materials. For example, nonvolatile polycyclic aromatic hydrocarbons and kerogen-like macromolecular carbon are found in some carbonaceous meteorites, which derived from asteroid parent bodies. A single focused laser pulse is able to volatilize and ionize some of these compounds for direct TOF analysis. While this is possible without any sample preparation or contact, sensitivity and quantitative performance can improve significantly with some sample handling. As such we have also been examining robotic mechanisms and protocols to accompany space flight mass spectrometers. In addition, sensors in early development may significantly improve these capabilities, via use of techniques such as switchable polarity, ambient pressure, or resonant ionization; tandem mass spectrometry (TOF or ion trap); and chemical imaging.

Brinckerhoff, William↗
NASA NTRS1993

Effect of Trapped Ions in a Gated Time-of-Flight Apparatus

K.E. Martus,O.J. Orient,A Three-mesh gate is used in a time-of-flight(TOF) apparatus to analyze the Velocity of positive ions. Test results and a theoretical description are presented of an effect arising from trapping ions between meshes of a two gate TOF velocity analyzer. The entrapped ions produce a side peak in the TOF spectra corresponding to faster ions.

time-of-flight↗
NASA NTRSDate not supplied

Ruggedizing a Commercial Depth Camera for Novel Lunar Exploration.

The novel contribution of this instrument is to take the first depth images on the moon. A commercial Kinect camera from Microsoft has been ruggedized for a CLPS mission to the Lunar South Pole. The 12-megapixel color camera is combined with a 1-megapixel color time-of-flight (ToF) depth sensor. The solid-state depth sensor/LIDAR provides greater resolution, a wider field of view, pixel binning, and reduced power consumption. The high-resolution data collected from the mission can be used to construct a near-field virtual environment of the lunar surface for scientific applications. The depth camera can provide a 360-degree view of the target area by combining ToF data with RGB imagery and rover turning. The unit was evaluated for space flight compliant materials and parts at NASA Ames. The microphone array, RF shield, front face, and outer body parts were removed to reduce mass. Plastic parts were replaced with vacuum-compatible materials; manufactured cables were added to properly interface with the host rover, built by Lunar Outpost. The environmental testing was performed on the Kinect with Random Vibration/Sine Testing (Fig 1a), per GEVS (NASA’s General Environmental Verification Standard for spaceflight launch survival). Thermal Vacuum testing cycled the instrument between expected hot (+ 85 C) and cold survival temperatures, as well as +50 C and -25 C operational temps (Fig 1b). The instrument functioned nominally at the conclusion of vibration and thermal cycling tests. The Azure Kinect is manifested on the Nova-C lander which flies on the Intuitive Machines mission IM-2, landing at the lunar south pole for a mission duration of 14 days (one lunar daylight cycle). The unit will be integrated to the MAPP (Mobile Autonomous Prospecting Platform) rover at Lunar Outpost. The Azure Kinect with ToF feature will improve the resolution of lunar geology data near the south pole and enable ground-based VR experience of details of the lunar surface (Fig 1c).

V. Jha↗
DOE OSTI2011

(237)Np(n,f) Cross Section: New Data and Present Status

In this document, we present the final result obtained at the n-TOF experiment for the neutron-induced fission cross section of the {sup 237}Np, from the fission threshold up to 1 GeV. The method applied to get this result is briefly discussed. n-TOF data are compared to the last experimental measurements using other TOF facilities or the surrogate method, reported experiments performed with monoenergetic sources and the FISCAL systematic, including a discussion about the existing discrepancies.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2018

Positron-emission tomography detector systems based on low-density liquid scintillators and precise time-resolving photodetectors

TOF-PET detector systems, and methods for imaging photon-emitting samples using the detector systems, are provided. The TOF-PET detector systems use large-area photodetectors with extremely high time-resolution and an approach to data collection and analysis that allows for the use of inexpensive low-density scintillator materials. The TOF-PET detector systems are characterized by their ability to identify, on a statistical basis, the transverse and depth location of the first of the series of energy deposition events that are generated when a gamma photon enters the low-density scintillator material.

Frisch, Henry J.↗
DOE OSTI2021

Multimodal imaging of oil-in-water bilgewater emulsion and biofilms

Bilgewater emulsions, consisting of oil and surfactant mixtures in water, affect many aquatic species. Thus development of methods and techniques to treat or mitigate the formation and undesired consequences of shipboard emulsions are urgently needed. This work presents new results of the evolution of the bilgewaer chemical and physical properties using in situ imaging. A Navy O/W emulsion consisting of three oils and a detergent mixture was used as the synthetic bilgewater model [1, 2]. Synthetic oil-in-water (O/W) emulsion droplets were seled in a vacuum compatible microfluidic sample holder and imaged using a suite of tools including scanning electron microscopy (SEM), time-of-flight secondary ion mass spectrometry (ToF-SIMS), confocal laser scanning microscopy, and optical microscopy, highlighting the advantage of multiscale analysis and its applications in waste reduction and treatment in the environment. The transferrable and vacuum compatible microfluidic interface, System for Analysis at the Liquid Vacuum Interface (SALVI), was used in this study. SALVI enabled surface analysis of liquids and liquid-solid interactions using ToF-SIMS and SEM [3, 4]. Its detection window is an aperture of 2 ?m in diameter open to vacuum, permitting direct detection of the liquid surface. Liquid is withheld by surface tension within the aperture. The interface is composed of a silicon nitride membrane and polydimethylsiloxane microchannel [3, 4]. A variety of samples including complex liquid mixtures, ionic liquids, single mammalian cells, live biofilms, and solid-electrolyte interface have been analyzed using in situ imaging [5, 6]. The feasibility of using SALVI for in situ SEM imaging of nanoparticles and colloids in liquid was recently demonstrated [7]. This paper shows new findings of multimodal imaging and analysis of synthesized emulsion particles in water. Figure 1 depicts a schematic of multimodal in situ imaging of bilgewater emulsion using SEM and ToF-SIMS. Furthermore, we study the interactions of microbes and bilgewater emulsion. Microbes play an important role in the ocean. We hypothesize that microbes release organics that can act as surfactants that affect bilgewater formation or weakening. We present the first systematic study of emulsions and biofilms and investigate the effects of biofilms on bilgewater emulsions. Pseudomonas was selected as a model strain. Biofilms were cultured in a microchannel to allow culture [8]. Once a thick layer of biofilms was formed, the medium solution was changed to a mixture consisting of 50 % bilgewater emulsion. Dispersed biofilms were collected at 24 hrs. and 48 hrs. after emulsions were introduced into the channel. Bilgewater emulsions, biofilms, and mixtures of bilgewater emulsions and biofilms were analyzed using multiple in situ and ex situ techniques as described earlier. Our findings indicate that biofilms change the chemical makeup of the emulsion surface compositions and emulsion droplet size distribution, confirming the hypothesis that extracellular polymeric substance (EPS) related components released from biofilms can function as surfactants and change the oil-in-water interfaces.

bilgewater, multimodal imaging, biofilms↗
DOE OSTI2022

Mass spectral imaging showing the plant growth-promoting rhizobacteria's effect on the Brachypodium awn

The plant growth-promoting rhizobacteria (PGPR) on the host plant surface play a key role in biological control and pathogenic response in plant functions and growth. However, it is difficult to elucidate the PGPR effect on plants. Such information is important in biomass production and conversion. Brachypodium distachyon (Brachypodium), a genomics model for bioenergy and native grasses, was selected as a C3 plant model; and the Gram-negative Pseudomonas fluorescens SBW25 ( P.) and Gram-positive Arthrobacter chlorophenolicus A6 ( A.) were chosen as representative PGPR strains. The PGPRs were introduced to the Brachypodium seed's awn prior to germination, and their possible effects on the seeding and growth were studied using different modes of time-of-flight secondary ion mass spectrometry (ToF-SIMS) measurements, including a high mass-resolution spectral collection and delayed image extraction. We observed key plant metabolic products and biomarkers, such as flavonoids, phenolic compounds, fatty acids, and auxin indole-3-acetic acid in the Brachypodium awns. Furthermore, principal component analysis and two-dimensional imaging analysis reveal that the Brachypodium awns are sensitive to the PGPR, leading to chemical composition and morphology changes on the awn surface. Our results show that ToF-SIMS can be an effective tool to probe cell-to-cell interactions at the biointerface. This work provides a new approach to studying the PGPR effects on awn and shows its potential for the research of plant growth in the future.

metabolite↗
DOE OSTI2020

Exploration of Electrochemical Reactions at Organic–Inorganic Halide Perovskite Interfaces via Machine Learning in In Situ Time-of-Flight Secondary Ion Mass Spectrometry

The instability of hybrid organic–inorganic perovskite (HOIP) devices is one of the significant challenges preventing commercialization. Exploring these phenomena is severely limited by the complexity of the intrinsic electrochemistry of HOIPs, the presence of multiple volatile and mobile ionic species, and the possible role of environmentally induced reactions at surfaces and triple-phase junctions. Here, in situ studies of the electrochemistry of methylammonium lead bromide perovskite with the Au electrode interface are reported via light- and voltage-dependent time-of-flight secondary ion mass spectrometry (ToF-SIMS) imaging of lateral perovskite heterostructures. While ToF-SIMS allows for the visualization of the chemical composition along the surface and its evolution with light and electrical bias, the interpretation of the multidimensional data obtained is often limited due to strong correlations between chemical signatures and the need to track multiple peaks at once. Here, a machine learning workflow combining the Hough transform and non-negative matrix factorization and no-negative tensor decomposition is developed to avoid this limitation and extract salient features of associated chemical changes and to separate the light- and voltage-dependent dynamics. Finally, combining these in situ characterizations and the machine learning workflow provides comprehensive information on the chemical nature of moving species, ion accumulation, and interfacial electrochemical reactions in HOIP devices.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Direct Characterization of Atomically Dispersed Catalysts: Nitrogen-Coordinated Ni Sites in Carbon-Based Materials for CO 2 Electroreduction

Metal, nitrogen-doped carbon materials have attracted interest as heterogenous catalysts that contain MN x active sites that are analogous to molecular catalysts. Of particular interest is Ni,N-doped carbon, a catalyst that is active for the electrochemical reduction of CO 2 to CO. Critical to the understanding of these materials is proof of single atomic sites and characterization of the environment surrounding the metal atom; however, directly probing this coordination remains challenging. This challenge is addressed in this study by combining scanning transmission electron microscopy (STEM), single atom electron energy loss spectroscopy (EELS), and time-of-flight secondary ion mass spectrometry (ToF-SIMS). Through STEM imaging, atomic dispersion of Ni in the carbon framework is confirmed and image analyses are utilized to give semiquantitative estimates of neighbor distance distributions and site densities of Ni atoms. Atomic resolution EELS demonstrates that N and Ni are colocated at the single Ni atom sites suggesting Ni–N coordination. ToF-SIMS reveals a distribution of NiN x C y - fragments that reflect the Ni–N bonding environments within Ni,N-doped carbon. The fragmentation from Ni,N-doped carbon is similar to Ni phthalocyanine, suggesting the existence of heterogenized, molecular-like NiN 4 active sites which motivates future studies that leverage insight from molecular catalysis design to develop next-generation heterogeneous catalysts.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2020

In situ liquid SIMS analysis of uranium oxide

Trace analysis of nuclear materials in solid particles collected in the environment or particles in liquid slurry generated in nuclear material manufacturing processes can pinpoint elemental, organic, and isotopic signatures of nuclear fuel cycle activities and processes. Such information can support nuclear safeguards programs by increasing our ability to detect undeclared nuclear materials, routine activities for safeguarding at declared facilities, and illicit activities. However, trace radioactive material analysis in liquids and slurries is challenging using bulk approaches. For example, one drawback of sensitive analysis such as inductively coupled plasma mass spectrometry (ICP-MS) is that sample is consumed or destroyed as a result of the technical approach. We developed a vacuum compatible microfluidic interface to enable surface analysis of liquids and liquid-solid interactions using time-of-flight secondary ion mass spectrometry (ToF-SIMS). In this work, we illustrate initial results of liquid standards containing uranium using in situ liquid SIMS. Specifically a series of diluted uranium standards used for ICPMS analysis were studied and the limit of detection was estimated. Since the liquid SIMS analysis is almost nondestructive, the same sample can be analyzed by other more destructive approaches afterwards or saved for future references. Consequently, multimodal analysis is possible. Our results demonstrate that in situ liquid SIMS can be used as a new approach to analyze radioactive materials in liquid and slurry forms of relevance to the IAEA safeguards missions.

In situ liquid ToF-SIMS, uranium, limit of detecti↗
DOE OSTI2018

Topochemical Understanding of Lignin Distribution During Hydrothermal Flowthrough Pretreatment

Changes in surface properties during biomass pretreatments are important parameters to understand and engineer biological biomass conversion processes. In particular, different influences on the surface of biomass are expected between flowthrough and batch pretreatments. In this paper, for a better understanding of biomass surface changes by hydrothermal flowthrough pretreatment, the mechanism by which the surface of biomass is altered in terms of cellulose and lignin was investigated using time-of-flight secondary ion mass spectrometry (ToF-SIMS) and compared with the bulk chemical composition and the results from scanning electron microscope (SEM). ToF-SIMS analysis results provide semi-quantitative information of cellulose and lignin and support the other observation from SEM and bulk compositional analyses. In brief, more lignin was observed on the surface of biomass at the early stage hydrothermal pretreatment, while the lignin mainly located at the cell corners was reduced by extended pretreatment time. Finally, unlike batch pretreatment, pseudo-lignin formation was not observed on the poplar surface during the flowthrough process.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2019

Application of time-of-flight secondary ion mass spectrometry to the detection of surface intermediates during the first cycle of atomic layer deposition (ALD) of platinum on silica surfaces

Atomic layer deposition (ALD) has become the method of choice for many applications requiring the controlled growth of thin films on solid surfaces. Yet, the use of metalorganic precursors typical in these depositions adds significant complexity to the chemistry involved. Unfortunately, it is difficult to obtain direct information about the surface species that participate in the reaction mechanisms of ALD. Here we illustrate the value of using time-of-flight secondary ion mass spectrometry (ToF-SIMS) for this purpose. A specific example is provided, a study of the first cycle of deposition of platinum using trimethyl(methylcyclopentadienyl)platinum (IV), or MeCpPt(CH 3 ) 3, on silicon oxide surfaces. In previous investigations of this process, we have determined that the low reactivity of the MeCpPt(CH 3 ) 3 precursor, which hinders fast deposition, can be partially overcome by gas-phase electron-impact activation. What has not been clear is what chemical species form on the solid surface as a result of such activation. Here we show that the MeCp ligand is quite stable and that it remains intact and coordinated to the Pt atoms upon adsorption on the surface. It was also established that some of the methyl groups may remain bound to the Pt center: the main species detected on the silicon oxide surfaces were MeCpPt and MeCpPt(CH 3 ). On the other hand, it appears that no Pt intermediates without MeCp ligands are formed during this initial adsorption. Finally, O 2 treatment of these surfaces at elevated temperature to complete the first ALD cycle leads to the complete removal of all the organic ligands: no evidence for MeCp or methyl groups is seen in the ToF-SIMS traces from the final samples.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2021

Ionizing photon interactions modulate the optical properties of crystals with femtosecond scale temporal resolution

In this work, we continue our study of a new method for the detection of ionizing radiation with the potential for a dramatic improvement in coincidence time resolution (CTR) for time-of-flight positron emission tomography (ToF-PET) using the modulation of a material's optical properties instead of the scintillation mechanism. Our previous work has shown that for non-scintillation materials such as bismuth silicon oxide (BSO) and cadmium telluride (CdTe), their refractive index can be modulated by annihilation photon interactions. Additionally, the ultrafast nature of this process however remains unexplored. The ionizing radiation-induced charge carriers alter the local band structure in these materials, thus changing the complex refractive index. This mechanism is routinely used at the linac coherent light source (LCLS) facility of the SLAC National Accelerator Laboratory to measure x-ray pulse arrival times with femtosecond scale resolution for photon energies between 0.5 and 10 keV. The method described here follows that example by using a frequency chirped visible continuum pulse to provide a monotonic wavelength-to-time mapping by which one can measure the time-dependent refractive index modulation. In addition, we describe an interference-based measurement setup that allows for significantly improved sensitivity while preserving a timing precision of approximately 10 fs (σ) when measuring the arrival time of below 10 keV x-ray pulses with yttrium aluminum garnet (YAG) crystal. The method is presented in the context of ToF-PET application with further discussions on the potential CTR achievable if a similar detection concept is adopted for detecting 511 keV photons. Semi-empirical analysis indicates that the predicted CTR achievable is on the order of 1 ps (FWHM).

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2018

A Novel Method to Investigate Stoichiometry and Performance of Buried Passivated Contacts Utilizing Time-of-Flight SIMS

We report on methods using time-of-flight secondary-ion mass spectrometry (TOF-SIMS) to elucidate critical information about the buried interfaces in interdigitated back-contact silicon solar cells. We examined the stoichiometry of the tunneling oxide with TOF-SIMS and X-ray photoelectron spectroscopy (XPS). Interestingly, the data indicates that the stoichiometry of the tunneling oxide moves away from SiO 2 towards lower stoichiometry (SiO x ) upon the crystallization annealing treatment, and towards SiO 2 again upon Al 2 O 3 deposition and a subsequent forming gas anneal. We also report on an important artifact for samples with an Al 2 O 3 passivation layer related to the oxygen content of the matrix.

14 SOLAR ENERGY↗