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At least 199 records · Page 11
All sourcesNASA NTRSDOE OSTI
NASA NTRS2001

Barium Isotopes in Single Presolar Grains

Barium isotopic compositions of single presolar grains were measured by laser ablation laser resonant ionization mass spectrometry and the implications of the data for stellar processes are discussed. Additional information is contained in the original extended abstract.

Pellin, M. J.↗
NASA NTRS2004

Fabricating Blazed Diffraction Gratings by X-Ray Lithography

Gray-scale x-ray lithography is undergoing development as a technique for fabricating blazed diffraction gratings. As such, gray-scale x-ray lithography now complements such other grating-fabrication techniques as mechanical ruling, holography, ion etching, laser ablation, laser writing, and electron-beam lithography. Each of these techniques offers advantages and disadvantages for implementing specific grating designs; no single one of these techniques can satisfy the design requirements for all applications. Gray-scale x-ray lithography is expected to be advantageous for making gratings on steeper substrates than those that can be made by electron-beam lithography. This technique is not limited to sawtooth groove profiles and flat substrates: various groove profiles can be generated on arbitrarily shaped (including highly curved) substrates with the same ease as sawtooth profiles can be generated on flat substrates. Moreover, the gratings fabricated by this technique can be made free of ghosts (spurious diffraction components attributable to small spurious periodicities in the locations of grooves). The first step in gray-scale x-ray lithography is to conformally coat a substrate with a suitable photoresist. An x-ray mask (see Figure 1) is generated, placed between the substrate and a source of collimated x-rays, and scanned over the substrate so as to create a spatial modulation in the exposure of the photoresist. Development of the exposed photoresist results in a surface corrugation that corresponds to the spatial modulation and that defines the grating surface. The grating pattern is generated by scanning an appropriately shaped x-ray area mask along the substrate. The mask example of Figure 1 would generate a blazed grating profile when scanned in the perpendicular direction at constant speed, assuming the photoresist responds linearly to incident radiation. If the resist response is nonlinear, then the mask shape can be modified to account for the nonlinearity and produce a desired groove profile. An example of grating grooves generated by this technique is shown in Figure 2. A maximum relative efficiency of 88 percent has been demonstrated.

Mouroulis, Pantazis↗
DOE OSTI2021

Features of ion generation by a picosecond laser in the range of 10 11 –10 13 W cm -2 power densities

Picosecond lasers (ps-lasers) have significant advantages for the generation of low charge state ions compared to nanosecond lasers because the influence of heat conductivity on a solid target is almost negligible in the case of ps-laser ablation for laser pulse durations less than 10 ps. However, there is no comprehensive data on ion yields for different elements and target irradiation conditions for laser power densities at the target surface around and below 10 13 W cm –2 , which is of interest to our study of such plasmas as a source of low charge state ions for various applications, particularly for external injection of those ions into an Electron Beam Ion Source (EBIS). We investigated ion generation from Al, Ti, Cu, Nb and Ta target elements by a ps-laser with power densities in the range of 10 11 –10 13 W cm –2 at the target surface. A ps-laser with 1.27 mJ maximum energy within an 8 ps pulse and repetition rate up to 400 Hz has been used to generate a laser-ablated plasma. Dependencies of ion current versus time, total charge of registered ions as well as ion kinetic energy distributions are characterized using a Faraday cup. Significant difference in ion current dynamics between first, second and following shots onto the same target spot was found for all five target elements. The total charge of ions registered by the Faraday cup increases linearly with increasing laser pulse energy and is almost independent of the target element and number of shots onto the same target spot for all five target elements studied. The results obtained give us a basis for specification and design of the source of low charge state ions for external injection into EBIS.

43 PARTICLE ACCELERATORS↗
DOE OSTI2023

Advancing Elemental and Isotopic Analysis of Uranium Mineral Inclusions: Rapid Screening via Laser-Induced Breakdown Spectroscopy and High-Resolution Laser Ablation-ICP-MS Mapping

The work presented herein employs two laser-based analytical techniques (laser-induced breakdown spectroscopy (LIBS) and laser ablation – inductively coupled plasma – mass spectrometry (LA-ICP-MS)) to spatially determine the elemental and isotopic composition of uranium bearing minerals. Uniquely, this work leverages the high-speed applicability of LIBS to “screen” the sample(s) for their elemental constituents. After determining the location of the uranium inclusions (via LIBS), high-resolution LA-ICP-MS was employed to further characterize the inclusions. The high-resolution (sub-µm) capabilities of LA-ICP-MS were able to extract important information from the uranium minerals including discerning its chemical form (e.g., finchite from carnotite, Sr- and K-bearing uranyl vanadates, respectively) as well as their 235 U/ 238 U isotopic composition. This approach, LIBS followed by LA-ICP-MS, significantly reduces the analysis time (~95 %) in comparison to employing a LA-ICP-MS only approach. Furthermore, this work presented a novel approach to analyzing inclusions via a particle/inclusion analysis tool which is commercially available within the iolite 4 software. This tool allowed for a more accurate characterization of the isotopic distribution of the inclusions, as well as allowing for rapid sizing of the inclusions. Finally, this analytical approach could readily be applied to other sample types in which the target species (e.g., µm-sized inclusions) are embedded in complex matrices (e.g., cm-sized samples).

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
NASA NTRS2012

In Situ Geochemical Analysis and Age Dating of Rocks Using Laser Ablation-Miniature Mass Spectrometer

A miniaturized instrument for performing chemical and isotopic analysis of rocks has been developed. The rock sample is ablated by a laser and the neutral species produced are analyzed using the JPL-invented miniature mass spectrometer. The direct sampling of neutral ablated material and the simultaneous measurement of all the elemental and isotopic species are the novelties of this method. In this laser ablation-miniature mass spectrometer (LA-MMS) method, the ablated neutral atoms are led into the electron impact ionization source of the MMS, where they are ionized by a 70-eV electron beam. This results in a secondary ion pulse typically 10-100 microsecond wide, compared to the original 5-10-nanosecond laser pulse duration. Ions of different masses are then spatially dispersed along the focal plane of the magnetic sector of the miniature mass spectrometer and measured in parallel by a modified CCD (charge-coupled device) array detector capable of detecting ions directly. Compared to conventional scanning techniques, simultaneous measurement of the ion pulse along the focal plane effectively offers a 100% duty cycle over a wide mass range. LAMMS offers a more quantitative assessment of elemental composition than techniques that detect laser-ionized species produced directly in the ablation process because the latter can be strongly influenced by matrix effects that vary with the structure and geometry of the surface, the laser beam, and the ionization energies of the elements. The measurement of high-precision isotopic ratios and elemental composition of different rock minerals by LAMMS method has been demonstrated. The LA-MMS can be applied for the absolute age determination of rocks. There is no such instrument available presently in a miniaturized version that can be used for NASA space missions. Work is in progress in the laboratory for geochronology of rocks using LA-MMS that is based on K-Ar radiogenic dating technique.

Sinha, Mahadeva P.↗
DOE OSTI2023

Faraday detector uranium isotope ratio measurement: Insights from solution- and laser ablation-based sampling methodologies on the Neoma MC-ICP-MS

In this study we utilize an all-faraday cup detector configuration on the Neoma MC-ICP-MS to perform uranium isotope ratio determinations from certified reference materials and a nuclear fuel precursor material via solution and laser ablation based sampling methodologies. The goal in performing these measurements is primarily to demonstrate that the all-faraday cup method can produce highly precise and accurate isotope ratios even at relatively low signal intensity levels while also developing a preliminary understanding of how the complex interplay between different amplifier resistor levels (e.g. 10 11 vs 10 13 Ω) and integration times impacts the precision and accuracy of different types of measurements. Our results show that the faraday cups with 1013 Ω resistors in their amplifier feedback loops can be used to produce accurate and relatively precise isotope ratios for ion beams down to ~5 K cps. However, at the lower end of the signal intensities observed in this study, longer integration times are necessary to mitigate the impact of ion beam instability that can occur during laser ablation based sampling. Despite this potential limitation, the all-faraday cup method is highly versatile as exemplified by the analysis of a collection of uranium reference materials with highly variable uranium isotopic compositions.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
DOE OSTI2021

Improved modeling of the solid-to-plasma transition of polystyrene ablator for laser direct-drive inertial confinement fusion hydrocodes

We report that the target performance of laser direct-drive inertial confinement fusion (ICF) can be limited by the development of hydrodynamic instabilities resulting from the nonhomegeneous laser absorption at the target surface, i.e., the laser imprint on the ablator. To understand and describe the formation of these instabilities, the early ablator evolution during the laser irradiation should be considered. In this work, an improved modeling of the solid-to-plasma transition of a polystyrene ablator for laser direct-drive ICF is proposed. This model is devoted to be implemented in hydrocodes dedicated to ICF which generally assume an initial plasma state. The present approach consists of the two-temperature model coupled to the electron, ion and neutral dynamics including the chemical fragmentation of polystyrene. The solid-to-plasma transition is shown to significantly influence the temporal evolution of both free electron density and temperatures, which can lead to different shock formation and propagation compared with an initial plasma state. The influence of the solid-to-plasma transition on the shock dynamics is evidenced by considering the scaling law of the pressure with respect to the laser intensity. The ablator transition is shown to modify the scaling law exponent compared with an initial plasma state.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Absolute quantitation of propranolol from 200-μm regions of mouse brain and liver thin tissues using laser ablation-dropletProbe-mass spectrometry

Rationale: The ability to quantify drugs and metabolites in tissue with sub-mm resolution is a challenging but much needed capability in pharmaceutical research. To fill this void, a novel surface sampling approach combining laser ablation with the commercial dropletProbe automated liquid surface sampling system (LA-dropletProbe) was developed and presented here.Methods: Parylene C-coated 200 × 200 μm tissue regions of mouse brain and kidney thin tissue sections were analyzed for propranolol by laser ablation of tissue directly into a preformed liquid junction. Propranolol was detected by high performance liquid chromatography with positive ion mode electrospray ionization tandem mass spectrometry. Quantitation was achieved via application of a stable isotope-labeled internal standard and an external calibration curve.Results: Absolute concentration of propranolol determined from 200 × 200 µm tissue regions were compared to propranolol concentrations obtained from 2.3-mm-diameter tissue punches of adjacent, non-coated sections using standard bulk tissue extraction protocols followed by regular HPLC-MS/MS analysis. Average concentration of propranolol in both organs determined by the two employed methods agreed within ±12%. Furthermore, the relative abundance of phase II hydroxypropranolol glucuronide metabolites were recorded and found to be consistent with previous results.Conclusions: This work illustrates that depositing a thin parylene C layer onto thin tissue prior to analysis, which seals the surface and prevents direct liquid extraction of the drug from the tissue, coupled to the novel LA-dropletProbe surface sampling system is a viable approach for sub-mm resolution quantitative drug distribution analysis.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2023

Laser Ablation-Capillary Absorption Spectroscopy: A novel approach for high throughput and increased spatial resolution measurements of δ 13 C in plant-soil systems

Spatial and temporal heterogeneity of nutrient exchange within the rhizosphere is a topic of increasing interest, although challenging to study due to limits in existing analytical capabilities. Here, we developed and demonstrated a new approach applying laser ablation sample introduction to capillary absorption spectroscopy (LA-CAS) to characterize carbon isotopic distribution within plant tissues, rhizosphere, and soil. We exposed switchgrass plants to 13 CO 2 to allow tracing of 13 C-labelled photosynthates within plant biomass and into the associated soil. The LA-CAS methods we describe leverage continuous measurements of a sample stream derived from laser ablation line scans (10-25 µm in width) over a sample surface which enables the user to produce an isotope map with a) higher data density or b) over larger spatial areas versus previously existing techniques. This versatility of LA-CAS is assessed through testing of a range of laser parameters (spot size, scan rates) on various materials (soil, plant biomass/tissues, and rhizosphere). Here, we demonstrate the ability of LA-CAS to provide near instantaneous $δ$ 13 C measurements over isotopically distinct surfaces to enable high spatially resolved mapping of 13 C-labelled material within the rhizosphere. Applying LA-CAS analysis to plant biomass, we observed higher $δ$ 13 C values concentrated within phloem structures, consistent with localized photosynthate transport. When mapping across the rhizosphere, 13 C-enriched soil was typically present within 5-10µm of root boundaries with a steep spatial increase in $δ$ 13 C when the scan approached the middle of the root. As with all LA approaches, care is required to ensure accurate results as phenomena linked to ablation, combustion, and isotopic measurement can impart artifacts if not carefully controlled. Still, taken as a whole, our demonstrations highlight the increased sample throughput, improved data density, and enhanced $δ$ 13 C capability of LA-CAS versus other LA techniques and emphasize the role this method can play in future plant and rhizosphere related studies.

59 BASIC BIOLOGICAL SCIENCES↗
NASA NTRS2018

Tandem LA-ICP-MS & LIBS; A New Micro-Analytical Technique for the Measurement of Every Element in the Periodic Table

Laser Ablation ICP-MS (LA-ICP-MS) has been widely accepted as a microanalytical technique for in-situ trace (ppb) elemental analysis on the micron scale in a variety of geologic materials. LA-ICP-MS (single or multi-collector) provides both elemental and isotopic measurements critical for a wide range of geological research by generating a fine grained aerosol (nm scale) during the laser ablation event and delivering that aerosol to the ICP ion source of the mass spectrometer via an inert carrier gas. LA-ICP-MS, however, suffers from limitations in analyzing high ionization potential elements as well as elements subject to atmospheric and argon based interferences. LA-ICP-MS also has limitations in analyzing major elements due to detector saturation. An alternative laser ablation technique, Laser Induced Breakdown Spectroscopy (LIBS), employs an optical spectrometer integrated into the laser ablation system that analyzes the laser induced plasma at the sample surface across the entire optical spectrum for emission lines of every element in the periodic table. Elements that are difficult or impossible to measure with LA-ICP-MS are now possible to analyze with LIBS down to low ppm levels with CCD and/or ICCD detection. We introduce a new laser based technique, “Tandem LA-LIBS”, that combines LA for ICP-MS and LIBS into one integrated laser ablation system. This system has the effect of expanding the elemental coverage and the dynamic range of the laser ablation experiment as measurements from ppb to % level matrix elements can now be analyzed in a single ablation experiment. We present both femtosecond and nanosecond Tandem LA-LIBS quantitative and qualitative data on wide range of geological materials for those elements that are difficult or impossible by traditional LA-ICP-MS techniques such as F, H, O, N, C, S, halogens, etc. We also demonstrate that the simultaneous measurement of trace, minor and major elements are now possible in a single laser ablation experiment with Tandem LA-LIBS technology.

LA-ICP-MS↗
DOE OSTI2020

The role of ambient gas confinement, plasma chemistry, and focusing conditions on emission features of femtosecond laser-produced plasmas

Ultrafast laser ablation coupled with optical emission spectroscopy is currently under development for standoff detection of elements and their isotopes for a wide range of application areas. In this work, we explore the role of ambient air pressure during the interaction of an ultrafast laser beam with two metallic targets (brass and uranium) with significantly different oxygen gas-phase reactivity. Plasma plumes were generated by focusing ~800 nm, ~35 fs pulses from an ultrafast laser system using a long focal length lens with f = 1 m. Two-dimensional spectral imaging was performed over the pressure range of 30 mTorr-700 Torr air to evaluate emission dynamics, plasma chemistry, signal-to-background ratio, and characteristic parameters (i.e. excitation temperature, electron density). An increase in ambient air pressure during ultrafast laser ablation leads to plume confinement and subsequent changes in the emission dynamics due to plasma chemistry as well as changes in plasma generation conditions (i.e. focused fs laser ablation versus filament ablation). Ablation crater morphologies were also investigated via scanning electron microscopy. Results indicate atomic emission intensity and signal-to-background ratios peak at moderate pressure levels (~50-100 Torr air) for both targets studied, although plasma chemistry influences uranium emission signatures. The emission features of the uranium plasma at pressures = 10 Torr showed the presence of atoms and oxide molecules which are co-located within the plume. We also find filament ablation leads to wider, more shallow craters compared to focused laser ablation. Our study provides unique insight into the interplay between plume dynamics, confinement, and oxygen chemistry of fs laser-produced plasmas and how these phenomena evolve with changing ambient air pressure.

Laser-produced plasma↗