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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 73 records · Page 4
All sourcesNASA NTRSDOE OSTI
DOE OSTI2024

In-house synthesized poly(ether ether ketone) ionenes. II. ToF-SIMS spectra in the negative ion mode

Time-of-flight secondary ion mass spectrometry (ToF-SIMS) was used to analyze poly(ether ether ketone) (PEEK) based membranes. PEEK membranes have been shown to be effective in the separation of CO 2 from flue gases (post-combustion technique). The PEEK membranes were synthesized using novel aromatic ether-ketone linkages inspired by PEEK with polymeric backbone bistriflimide [Tf2N]− counterions. One of the keys to advancing this technology is developing membranes that are selective and permeable toward CO 2 , in which PEEK based membranes have been shown to be. Furthermore, the compatibility between various water lean solvents also needs to be investigated. Surface analytical techniques such as x-ray photoelectron spectroscopy and ToF-SIMS are useful for investigating chemical changes between membranes. Herein, we present ToF-SIMS data obtained in the negative ion mode for four different PEEK membranes designed for use in CO 2 capture systems. Positive ion mode spectra are reported in Paper I.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2011

LC-IM-TOF Instrument Control & Data Visualization Software

Liquid Chromatography-Ion Mobility-time of Flight Instrument Control and Data Visualization software is designed to control instrument voltages for the Ion Mobility drift tube. It collects and stores information collected from the Agilent TOF instrument and analyses/displays the ion intensity information acquired. The software interface can be split into 3 categories -- Instrument Settings/Controls, Data Acquisition, and Viewer. The Instrument Settings/Controls prepares the instrument for Data Acquisition. The Viewer contains common objects that are used by Instrument Settings/Controls and Data Acquisition. Intensity information is collected in 1 nanosec bins and separated by TOF pulses called scans. A collection of scans are stored side by side making up an accumulation. In order for the computer to keep up with the stream of data, 30-50 accumulations are commonly summed into a single frame. A collection of frames makes up an experiment. The Viewer software then takes the experiment and presents the data in several possible ways, each frame can be viewed in TOF bins or m/z (mass to charge ratio). The experiment can be viewed frame by frame, merging several frames, or by viewing the peak chromatogram. The user can zoom into the data, export data, and/or animate frames. Additional features include calibration of the data and even post-processing multiplexed data.

Danielson III, WilliamF.↗
DOE OSTI2022

Interrogating organo-mineral interactions by Py-GC/MS and ToF-SIMS

Soil organic matter (SOM) is crucial to soil fertility and agricultural sustainability in the face of climate change, and organo-mineral interactions are a key mechanism for stabilizing SOM. The stability of mineral-associated organic matter (MAOM) can be approximated by the strength of bonds between biomolecules and mineral surfaces. We hypothesized that factors such as mineral reactivity and solution pH would impact bonding strength. To test these factors, sorption isotherms were performed on minerals differing in particle size, morphology, and reactivity (quartz, goethite, gibbsite, kaolinite, montmorillonite), under two pH conditions (4 and 6), and across a range of tannic acid concentration (0-1400 ppm). The quantity and quality of organo-mineral bonds was assessed by quantifying post-sorption solution compounds using an absorbance plate reader and assessing the thermal energy needed to break bonds using evolved gas analysis (EGA) on a pyrolysis gas chromatograph-mass spectrometer (Py-GC/MS). Organo-mineral surfaces were also interrogated using Time-of-flight secondary ion mass spectrometry (ToF-SIMS). Sorption experiments revealed an asymptotic relationship between sorbed tannic acid and increasing initial concentrations which suggests our concentration range saturated available mineral surfaces. Results indicated that mineral identity, chiefly surface area and native pH, impacted the amount of compound sorbed to mineral surfaces. Evolved gas analyses of organo-mineral samples uncovered increased thermal stability of sorbed compounds compared to our tannic acid standard particularly on the iron oxide, goethite. ToF-SIMS revealed that goethite surface ions were covered by increasing concentrations of adsorbed tannic acid with the replacement of chlorine and sulfate ions by tannic acid related ions. Our results indicate that Py-GC/MS and ToF-SIMS are useful techniques to determine the nature and strength of organo-mineral bonds and are steppingstones to understanding controls on carbon sequestration in terrestrial systems.

58 GEOSCIENCES↗
DOE OSTI2019

A method for extracting calibrated volatility information from the FIGAERO-HR-ToF-CIMS and its experimental application

The Filter Inlet for Gases and AEROsols (FIGAERO) is an inlet specificallydesigned to be coupled with the Aerodyne High-Resolution Time-of-FlightChemical Ionization Mass Spectrometer (HR-ToF-CIMS). The FIGAERO-HR-ToF-CIMSprovides simultaneous molecular information relating to both the gas- andparticle-phase samples and has been used to extract vapour pressures (VPs) ofthe compounds desorbing from the filter whilst giving quantitativeconcentrations in the particle phase. However, such extraction of vapourpressures of the measured particle-phase components requires use ofappropriate, well-defined, reference compounds. Vapour pressures for thehomologous series of polyethylene glycols (PEG)((H-(O-CH 2 -CH 2 )n-OH) for n=3 to n=8), covering a rangeof vapour pressures (VP) (10 -1 to 10 -7 Pa) that areatmospherically relevant, have been shown to be reproduced well by a range ofdifferent techniques, including Knudsen Effusion Mass Spectrometry (KEMS).This is the first homologous series of compounds for which a number of vapourpressure measurement techniques have been found to be in agreement,indicating the utility as a calibration standard, providing an ideal set ofbenchmark compounds for accurate characterization of the FIGAERO forextracting vapour pressure of measured compounds in chambers and the realatmosphere. To demonstrate this, single-component and mixture vapour pressuremeasurements are made using two FIGAERO-HR-ToF-CIMS instruments based on anew calibration determined from the PEG series. VP values extracted from bothinstruments agree well with those measured by KEMS and reported values fromliterature, validating this approach for extracting VP data from the FIGAERO.This method is then applied to chamber measurements, and the vapour pressuresof known products are estimated.

47 OTHER INSTRUMENTATION↗
NASA NTRS2002

MALDI TOF MS: An Exobiology Surface-Science Approach for Europa

If Europa is to be of primary exobiological interest, namely as a habitat for extant life, it is obvious that: (i) a hydrosphere must prevail beneath the cryosphere for a long time, (ii) internal energy sources must be present in a sufficient state of activity, and (iii) a reasonable technical means must be available for assessing if indeed life does exist in the hypothesized hydrosphere. This discussion focuses on technological issues, because the compounding evidence about Europa indicates that the first two are highly likely to be true. We present a consideration of time-of-flight mass spectroscopy (TOF MS) conducted in-situ on the cryosphere surface of Europa during a landed robotic mission. We assert that this is a reasonable technical means not only for exploring the composition of the cryosphere itself, but also for locating any biomolecular indicators of extant life brought to the surface through cryosphere activity. We also describe a MALDI (MAtrix Laser Desorption and Ionization) TOF MS system that we are constructing as a proof-of-concept prototype for conducting TOF MS measurements on Europa.

Gerakines, Perry A.↗
NASA NTRS2003

"DUST BUSTER" - A Single Photon Ionization TOF MS for Cometary Dusts

It is hard to predict the properties and composition of dust that will be returned by STARDUST from WED- 2. The most interesting but challenging case would be grains, pg to fg in weight, each carrying its own isotopic signature characteristic of its source zones in a variety of stars. How do we extract the maximum amount of science from such grains? Clearly, the best that can be accomplished is to measure every atom in each grain.Academia Sinica and Argonne National Laboratory (ANL) have entered into a collaboration to develop a SPI TOF MS instrument for analysis of stardust grains. A new instrument will be built at Academia Sinica based on the new TOF mass spectrometer design developed, built and operating at ANL. The instrument is intended for SPI TOF MS analysis of elements from Ca to Cu plus Li after first using SIMS to measure H, C, N, 0, Si, and S. There are still technical challenges facing the technique. We will need to improve submicrometer sample handling, avoid the effects of space charge, and increase the Mamie range of the detector. The most difficult obstacle to overcome may be the fact that the flux density of present high repetition rate, WV lasers is below the level needed to ensure full ionization (saturation) in the source region, which must be several mm in size to achieve the high useful yield needed for analysis of small stardust grains. A potential breakthrough effort is to exploit the novel free electron laser being pioneered at ANL. In principle, this FEL can reach ionization saturation and is tunable up to photon energies of 25 eV, which is higher than the ionization potential of any element.

Chen, C.-Y.↗
NASA NTRS2006

Spontaneous-Desorption Ionizer for a TOF-MS

A time-of-flight mass spectrometer (TOF-MS) like the one mentioned in the immediately preceding article has been retrofitted with an ionizer based on a surface spontaneous-desorption process. This ionizer includes an electron multiplier in the form of a microchannel plate (MCP). Relative to an ionizer based on a hot-filament electron source, this ionizer offers advantages of less power consumption and greater mechanical ruggedness. The current density and stability characteristics of the electron emission of this ionizer are similar to those of a filament-based ionizer. In tests of various versions of this ionizer in the TOF-MS, electron currents up to 100 nA were registered. Currents of microamperes or more - great enough to satisfy requirements in most TOFMS applications - could be obtained by use of MCPs different from those used in the tests, albeit at the cost of greater bulk. One drawback of this ionizer is that the gain of the MCP decreases as a function of the charge extracted thus far; the total charge that can be extracted over the operational lifetime is about 1 coulomb. An MCP in the ion-detector portion of the TOF-MS is subject to the same limitation.

Schultz, J. Albert↗
DOE OSTI2011

Fission Cross-section Measurements of (233)U, (245)Cm and (241,243)Am at CERN n_TOF Facility

Neutron-induced fission cross-sections of minor actinides have been measured using the n-TOF white neutron source at CERN, Geneva, as part of a large experimental program aiming at collecting new data relevant for nuclear astrophysics and for the design of advanced reactor systems. The measurements at n-TOF take advantage of the innovative features of the n-TOF facility, namely the wide energy range, high instantaneous neutron flux and good energy resolution. Final results on the fission cross-section of {sup 233}U, {sup 245}Cm and {sup 243}Am from thermal to 20 MeV are here reported, together with preliminary results for {sup 241}Am. The measurement have been performed with a dedicated Fast Ionization Chamber (FIC), a fission fragment detector with a very high efficiency, relative to the very well known cross-section of {sup 235}U, measured simultaneously with the same detector.

79 ASTRONOMY AND ASTROPHYSICS↗
DOE OSTI2011

Measurement of the (236)U(n,f) cross section from 170 MeV to 2 MeV at the CERN n_TOF Facility

The neutron-induced fission cross section of {sup 236}U was measured at the neutron Time-of-Flight (n-TOF) facility at CERN relative to the standard {sup 235}U(n,f) cross section for neutron energies ranging from above thermal to several MeV. The measurement, covering the full range simultaneously, was performed with a fast ionization chamber, taking advantage of the high resolution of the n-TOF spectrometer. The n-TOF results confirm that the first resonance at 5.45 eV is largely overestimated in some nuclear data libraries. The resonance triplet around 1.2 keV was measured with high resolution and resonance parameters were determined with good accuracy. Resonances at high energy have also been observed and characterized and different values for the cross section are provided for the region between 10 keV and the fission threshold. The present work indicates various shortcomings of the current nuclear data libraries in the subthreshold region and provides the basis for an accurate re-evaluation of the {sup 236}U(n,f) cross section, which is of great relevance for the development of emerging or innovative nuclear reactor technologies.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗
DOE OSTI2011

Probing the Orientation of Surface-Immobilized Protein G B1 Using ToF-SIMS Sum Frequency Generation and NEXAFS Spectroscopy

The ability to orient active proteins on surfaces is a critical aspect of many medical technologies. An important related challenge is characterizing protein orientation in these surface films. This study uses a combination of time-of-flight secondary ion mass spectrometry (ToF-SIMS), sum frequency generation (SFG) vibrational spectroscopy, and near-edge X-ray absorption fine structure (NEXAFS) spectroscopy to characterize the orientation of surface-immobilized Protein G B1, a rigid 6 kDa domain that binds the Fc fragment of IgG. Two Protein G B1 variants with a single cysteine introduced at either end were immobilized via the cysteine thiol onto maleimide-oligo(ethylene glycol)-functionalized gold and bare gold substrates. X-ray photoelectron spectroscopy was used to measure the amount of immobilized protein, and ToF-SIMS was used to measure the amino acid composition of the exposed surface of the protein films and to confirm covalent attachment of protein thiol to the substrate maleimide groups. SFG and NEXAFS were used to characterize the ordering and orientation of peptide or side chain bonds. On both substrates and for both cysteine positions, ToF-SIMS data showed enrichment of mass peaks from amino acids located at the end of the protein opposite to the cysteine surface position as compared with nonspecifically immobilized protein, indicating end-on protein orientations. Orientation on the maleimide substrate was enhanced by increasing pH (7.0-9.5) and salt concentration (0-1.5 M NaCl). SFG spectral peaks characteristic of ordered {alpha}-helix and {beta}-sheet elements were observed for both variants but not for cysteine-free wild type protein on the maleimide surface. The phase of the {alpha}-helix and {beta}-sheet peaks indicated a predominantly upright orientation for both variants, consistent with an end-on protein binding configuration. Polarization dependence of the NEXAFS signal from the N 1s to {pi}* transition of {beta}-sheet peptide bonds also indicated protein ordering, with an estimated tilt angle of inner {beta}-strands of 40-50{sup o} for both variants (one variant more tilted than the other), consistent with SFG results. The combined results demonstrate the power of using complementary techniques to probe protein orientation on surfaces.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2026

Combining ToF‐SIMS and Multivariate Analysis to Resolve Active Sites on Ni‐Based HER Catalysts

Unambiguous identification of active sites in heterogeneous catalysis remains a major challenge, particularly for materials with ultrathin, chemically mixed surface layers. Here, we demonstrate a generalizable approach that combines time-of-flight secondary ion mass spectrometry (ToF-SIMS) with multivariate statistical analysis (principal component analysis [PCA] and multivariate curve resolution [MCR]) to resolve catalytically relevant motifs at the nanoscale. Using Ni electrodes as a model system, PCA distinguished hydroxide-enriched domains from oxide- and metal-rich regions, while MCR decomposed depth profiles and 3D images into hydroxide, oxide, and metallic layers with nanometer resolution. A unique secondary-ion fragment, NiO 3 H 3 − (m/z 108.94), emerged as a marker of hydroxide-rich environments and correlated with hydrogen evolution reaction (HER) activity across a series of Ni electrodes. Complementary density functional theory (DFT) calculations revealed that Ni(OH) 2 clusters adjacent to metallic Ni offer the most favorable water dissociation energetics, establishing the structural origin of the marker. While illustrated here for Ni-based HER, this workflow provides a broadly applicable framework to isolate and rank near-surface patterns that govern catalytic activity, thereby extending ToF-SIMS from a qualitative probe to a predictive tool for active site identification.

HER active sites↗
DOE OSTI2012

An Investigation of Hydrogen Depth Profiling Using ToF-SIMS

Hydrogen depth distributions in silicon, zinc oxide and glass are of great interest in material research and industry. Time-of-flight secondary ion mass spectrometry (ToF-SIMS) has been used for hydrogen depth profiling for many years. However, some critical information, such as optimal instrumental settings and detection limits, is not easily available from previous publications. In this work, optimal instrumental settings and detection limits of hydrogen in silicon, zinc oxide and common glass were investigated. The recommended experimental settings for hydrogen depth profiling using ToF-SIMS are: (1) keeping pressure in the analysis chamber as low as possible, (2) using a cesium beam for sputtering and monitoring the H{sup -} signal, (3) employing monatomic ion analysis beams with the highest currents, and (4) using interlace mode. In addition, monatomic secondary ions from a matrix are recommended as references to normalize the H{sup -} signal. Detection limits of hydrogen are limited by pressure of residual gases in the analysis chamber. The base pressure of the analysis chamber (with samples) is about 7 x 10{sup -10} mbar in this study, and the corresponding detection limits of hydrogen in silicon, zinc oxide, and common glass are 1.3 x 10{sup 18} atoms/cm{sup 3}, 1.8 x 10{sup 18} atoms/cm{sup 3}, and 5.6 x 10{sup 18} atoms/cm{sup 3}, respectively.

08 HYDROGEN↗
DOE OSTI2014

In situ SEM and ToF-SIMS analysis of IgG conjugated gold nanoparticles at aqueous surfaces

In this study, we report new results of in situ study of 5 nm goat anti-mouse IgG gold nanoparticles in a novel portable vacuum compatible microfluidic device using scanning electron microscope (SEM) and time-of-flight secondary ion mass spectrometry (ToF-SIMS). The unique feature of the liquid flow cell is that the detection window is open to the vacuum allowing direct probing of the liquid surface. The flow cell is composed of a silicon nitride (SiN) membrane and polydimethylsiloxane (PDMS), and it is fully compatible with vacuum operations for surface analysis. The aperture can be drilled through the 100 nm SiN membrane using a focused ion beam. Characteristic signals of the conjugated gold nanoparticles were successfully observed through the aperture by both energy-dispersive X-ray spectroscopy (EDX) in SEM and ToF-SIMS. Comparison was also made among wet samples, dry samples, and liquid sample in the flow cell using SEM/EDX. Stronger gold signal can be observed in our novel portable device by SEM/EDX compared with the wet or dry samples, respectively. Our results indicate that analyses of the nanoparticle components are better made in their native liquid environment. This is made possible using our unique microfluidic flow cell.

aqueous surface↗
DOE OSTI2016

Nanoscale imaging of Li and B in nuclear waste glass, a comparison of ToF-SIMS, NanoSIMS, and APT: Nanoscale imaging of Li and B in nuclear waste glass

It has been very difficult to use popular elemental imaging techniques to image Li and B distribution in glass samples with nanoscale resolution. In this study, atom probe tomography (APT), time-of-flight secondary ion mass spectrometry (ToF-SIMS), and nanoscale secondary ion mass spectrometry (NanoSIMS) were used to image the distribution of Li and B in two representative glass samples. APT can provide three-dimensional Li and B imaging with very high spatial resolution (≤ 2 nm). In addition, absolute quantification of Li and B is possible, though room remains to improve accuracy. However, the major drawbacks of APT include limited field of view (normally ≤ 100 × 100 × 500 nm 3 ) and poor sample compatibility. As a comparison, ToF-SIMS and NanoSIMS are sample-friendly with flexible field of view (up to 500 × 500 μm 2 and image stitching is feasible); however, lateral resolution is limited to only about 100 nm. Therefore, SIMS and APT can be regarded as complementary techniques for nanoscale imaging Li and B in glass and other novel materials.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2024

ToF-SIMS in material research: A view from nanoscale hydrogen detection

Hydrogen in materials has attracted tremendous interest as its incorporation leads to significant alterations in nanoscale structure, composition, and chemistry, impacting functional properties. It has also been integral to nuclear fusion reactors and is considered a future clean energy source. However, nanoscale characterization and manipulation of hydrogen in materials are challenging as only a selected few analytical techniques can readily detect hydrogen, among which time-of-flight secondary ion mass spectrometry (ToF-SIMS) is a unique and powerful one due to its excellent detection limit along with decent depth and lateral resolutions. Here, in this review, we discuss, using selected examples, how to detect and quantify hydrogen in materials by ToF-SIMS and its impact on revealing the hydrogenation/protonation-induced novel functional states in different classes of materials. In addition, we present our protocols on sample preparation and experimental conditions optimization, allowing us to achieve the best possible results. Finally, we highlight future research directions that can lead to the discovery of novel functional states and ultimately provide a deeper understanding of scientific questions in materials science.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Study of cluster ions produced from ToF-SIMS analysis of a U-6%Nb target

Cluster ions have been previously observed during time-of-flight secondary ion mass spectrometry (ToF-SIMS) analysis of metals and metal oxides. Furthermore, we have used ToF-SIMS to investigate cluster ions formed from the hydrocarbon-containing overlayer, the mixed U and Nb surface oxide, and underlying metal of a U-6 %Nb (U6Nb) target. In the overlayer, we observe U x O y + oxides and U-species likely containing hydrocarbons. In the surface oxide, we observe UO 2 +, U 2 O 2 +, U 3 O 5 +, and U 4 O 6 + as the most intense ions for each family of oxide ions containing x U atoms. Nb oxides for NbO 1-2 - were only observed in negative polarity. In contrast to the oxide, analysis of the underlying U6Nb alloy resulted in repeating units of U n +, U n (Nb)+, and U n (Nb 2 ) + ions for n = 3–11 as the highest intensity ions for each family of ions containing n U atoms. Nb n + clusters were not observed. U n +, U n (Nb)+, and U n (Nb 2 )+ clusters containing C- and O-species were observed and were likely produced from soluble C or O species or precipitates known to be present in U6Nb.

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

Molecular Determination of Organic Adsorption Sites on Smectite during Fe Redox Processes Using ToF-SIMS Analysis

Turnover of soil organic carbon (SOC) is strongly affected by a balance between mineral protection and microbial degradation. However, the mechanisms controlling the heterogeneous and preferential adsorption of different types of SOC remain elusive, especially for humic substrates (HSs) and microbial carbon (MC), two hotly-debated forms of SOC prevalent in soils. In this work, the heterogeneous adsorption of HSs and MC on a clay mineral (nontronite NAu-2) during microbial-mediated Fe redox cycling was determined with the use of time-of-flight secondary ion mass spectrometry (ToF-SIMS). The results revealed that HSs pre-adsorbed on NAu-2 would partially inhibit the microbial Fe(III) reduction and structural modification of NAu-2, thus retarding the subsequent adsorption of MC. In contrast, NAu-2 without pre-coated HSs was adsorbed by a significant amount of MC from microbial polysaccharides as a result of Fe(III) reduction. This was attributed to the deposition of a thin Al-rich layer on clay surface, which provided active sites for MC adsorption. This study provides direct and detailed molecular evidence for the first time to explain the preferential adsorption of MC over HSs on the surface of clay minerals in the iron redox processes, which could be critical for the preservation of MC in soil. The results also indicate that ToF-SIMS is a unique tool for understanding complex organic-mineral-microbe interactions.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2018

Understanding Chemical Inhomogeneities and Cation Gradients in Perovskite Photovoltaics with TOF-SIMS

Time-of-flight secondary-ion mass spectrometry (TOF-SIMS) is one of the few techniques that can obtain chemical information from all components of hybrid organic-inorganic perovskite photovoltaics in up to three dimensions. This can yield critical insight into the uniformity of the cations through the thickness of the film (with sub-nm resolution), as well as laterally (with 100nm resolution) We have been using a TOF-SIMS to analyze perovskite photovoltaics at NREL for more than four years and have found many tricks and best practices, summarized here, to get around known artifacts when depth profiling and imaging.

14 SOLAR ENERGY↗