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At least 1,441 records · Page 80
All sourcesNASA NTRSDOE OSTI
DOE OSTI2024

Autonomous Synthesis of Thin Film Materials with Pulsed Laser Deposition Enabled by In Situ Spectroscopy and Automation

Autonomous systems that combine synthesis, characterization, and artificial intelligence can greatly accelerate the discovery and optimization of materials, however platforms for growth of macroscale thin films by physical vapor deposition techniques have lagged far behind others. Here this study demonstrates autonomous synthesis by pulsed laser deposition (PLD), a highly versatile synthesis technique, in the growth of ultrathin WSe 2 films. Further, by combing the automation of PLD synthesis and in situ diagnostic feedback with a high-throughput methodology, this study demonstrates a workflow and platform which uses Gaussian process regression and Bayesian optimization to autonomously identify growth regimes for WSe 2 films based on Raman spectral criteria by efficiently sampling 0.25% of the chosen 4D parameter space. With throughputs at least 10x faster than traditional PLD workflows, this platform and workflow enables the accelerated discovery and autonomous optimization of the vast number of materials that can be synthesized by PLD.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Physical conditions for UO formation in laser-produced uranium plumes

Laser-induced plasma spectroscopy is a powerful method for elemental detection and analysis, however the broadening and merging of densely packed spectral lines can make it especially challenging for studying high-Z elements such as uranium and other actinides. In order to understand the processes occurring in laser-induced plasma, it is necessary to evaluate the variation of its thermodynamic parameters. We performed spatiotemporal diagnostics of uranium species in plasma plumes produced by nanosecond near-infrared laser pulses in low- pressure environment. Spatially- and temporally-resolved emission spectroscopy experiments are supported by modeling of uranium emission and its persistence in the plume. Saha-Eggert equation as well as Boltzmann diagrams generated from numerous U I transitions are used to infer temperature. We report the rst measurements of uranium Stark broadening parameters for U I 499.01 nm and U II 500.82 nm transitions. The Stark widths of selected U transitions were measured by comparing their linewidths with the broadening of O I 777.19 nm line. Electron density was found to be on the order of 1016 cm??3, while the temperature was found to be in the range of 3000{8000 K. In addition to enhancing the fundamental understanding of high-Z plasmas under reduced-pressure environments, the knowledge of Stark broadening parameters could improve modeling capabilities and analytical performance of techniques that rely on emission plasma spectroscopy.

(140.3440) Laser-induced breakdown, (280.4788) Opt↗
DOE OSTI2025

Gold L-shell emission spectroscopy as a temperature diagnostic in laser-driven experiments

Measurements of plasma conditions within gold hohlraums are challenging but provide important information about hohlraum energy transport. To date, there are no reliable passive diagnostic approaches that produce information about the hohlraum plasma conditions. Gold L-shell emission spectroscopy is a promising method to measure the electron temperature in multi-keV gold hohlraum plasmas. In this study, we compare time-resolved measurements of gold L-shell spectra against a more conventional electron temperature-sensitive diagnostic, K-shell emission from zinc, a mid-Z dopant. The Au L-shell and Zn K-shell spectra are taken simultaneously. The analysis of both sets of data exhibits good agreement with a singular rad-hydro model, suggesting a similar evolution in the mean electron temperature of the hohlraum plasma. These findings support the use of L-shell spectroscopy of gold as a method to study gold plasma conditions.

Emission spectroscopy↗
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 OSTI2018

Optical emission from ultrafast laser filament-produced air plasmas in the multiple filament regime

We perform optical emission spectroscopy of ultrafast laser filament-produced air plasmas in the multiple filament regime at driving wavelengths of 400 nm and 800 nm. The spatiotemporal structure of the emission from the plasmas are observed and the emission spectra are used to estimate plasma temperature and density for a range of laser parameters. Plasma temperatures are determined from the molecular nitrogen fluorescence, while the electron densities are estimated from Stark broadening of the oxygen-I 777.19-nm line. Electron temperatures are determined to be in the range of 5000–5200 K and they do not vary significantly along the length of the filament, nor are they sensitive to incident laser energy or wavelength. Electron densities are on order of 1016 cm-3 and show a greater variation with axial position, laser energy, and laser wavelength. We discuss mechanisms responsible for spatial localization of emitting species within the filament. Optical emission spectroscopy offers a simple, non-perturbing method to measure filament properties, that allows the information on the associated molecular transitions and excitation/ionization mechanisms to be extracted.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2014

Persistence of uranium emission in laser-produced plasmas

Detection of uranium and other nuclear materials is of the utmost importance for nuclear safeguards and security. Optical emission spectroscopy of laser-ablated U plasmas has been presented as a stand-off, portable analytical method that can yield accurate qualitative and quantitative elemental analysis of a variety of samples. In this study, optimal laser ablation and ambient conditions are explored, as well as the spatio-temporal evolution of the plasma for spectral analysis of excited U species in a glass matrix. Various Ar pressures were explored to investigate the role that plasma collisional effects and confinement have on spectral line emission enhancement and persistence. The plasma-ambient gas interaction was also investigated using spatially resolved spectra and optical time-of-flight measurements. The results indicate that ambient conditions play a very important role in spectral emission intensity as well as the persistence of excited neutral U emission lines, influencing the appropriate spectral acquisition conditions.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
DOE OSTI2013

Infrared Scattering Scanning Near-Field Optical Microscopy Using An External Cavity Quantum Cascade Laser For Nanoscale Chemical Imaging And Spectroscopy of Explosive Residues

Infrared scattering scanning near-field optical microscopy (s-SNOM) is an apertureless superfocusing technique that uses the antenna properties of a conducting atomic force microscope (AFM) tip to achieve infrared spatial resolution below the diffraction limit. The instrument can be used either in imaging mode, where a fixed wavelength light source is tuned to a molecular resonance and the AFM raster scans an image, or in spectroscopy mode where the AFM is held stationary over a feature of interest and the light frequency is varied to obtain a spectrum. In either case, a strong, stable, coherent infrared source is required. Here we demonstrate the integration of a broadly tunable external cavity quantum cascade laser (ECQCL) into an s-SNOM and use it to obtain infrared spectra of microcrystals of chemicals adsorbed onto gold substrates. Residues of the explosive compound tetryl was deposited onto gold substrates. s-SNOM experiments were performed in the 1260-1400 cm-1 tuning range of the ECQCL, corresponding to the NO2 symmetric stretch vibrational fingerprint region. Vibrational infrared spectra were collected on individual chemical domains with a collection area of *500nm2 and compared to ensemble averaged far-field reflection-absorption infrared spectroscopy (RAIRS) results.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
DOE OSTI2017

Soft x-ray absorption spectroscopy of metalloproteins and high-valent metal-complexes at room temperature using free-electron lasers

X-ray absorption spectroscopy at the L-edge of 3d transition metals provides unique information on the local metal charge and spin states by directly probing 3d-derived molecular orbitals through 2p-3d transitions. However, this soft x-ray technique has been rarely used at synchrotron facilities for mechanistic studies of metalloenzymes due to the difficulties of x-ray-induced sample damage and strong background signals from light elements that can dominate the low metal signal. Here, we combine femtosecond soft x-ray pulses from a free-electron laser with a novel x-ray fluorescence-yield spectrometer to overcome these difficulties. We present L-edge absorption spectra of inorganic high-valent Mn complexes (Mn ∼ 6–15 mmol/l) with no visible effects of radiation damage. We also present the first L-edge absorption spectra of the oxygen evolving complex (Mn4CaO5) in Photosystem II (Mn < 1 mmol/l) at room temperature, measured under similar conditions. Our approach opens new ways to study metalloenzymes under functional conditions.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2015

Experimental approaches for studying non-equilibrium atmospheric plasma jets

This work reviews recent research efforts undertaken in the area non-equilibrium atmospheric plasma jets with special focus on experimental approaches. Physics of small non-equilibrium atmospheric plasma jets operating in kHz frequency range at powers around few Watts will be analyzed, including mechanism of breakdown, process of ionization front propagation, electrical coupling of the ionization front with the discharge electrodes, distributions of excited and ionized species, discharge current spreading, transient dynamics of various plasma parameters, etc. Experimental diagnostic approaches utilized in the field will be considered, including Rayleigh microwave scattering, Thomson laser scattering, electrostatic streamer scatterers, optical emission spectroscopy, fast photographing, etc.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗
DOE OSTI2020

Laser-Induced Plasma as a Method for the Metallic Materials Hardness Estimation: An Alternative Approach

The application of an alternative laser-induced breakdown spectroscopy (LIBS) method based on transversely excited atmospheric (TEA) CO2 laser was investigated for the first time for estimating the hardness of metallic materials. The human eye-safe (TEA) CO2 laser, operating at 10.6 µm, was used for plasma generation. The LIBS spectra were recorded by employing a cost-effective CCD camera for the time-integrated and spatial resolved measurements. The cast iron and aluminum alloys samples with different hardness have been tested. The ratio between the magnesium ionic and neutral lines in LIBS spectra was applied for estimating the material hardness. In addition, the hardness of all samples included in this study was determined using the conventional method for material hardness determination, i.e. Vickers hardness test. The linear dependence of magnesium lines intensity ratio on the sample’s hardness was obtained for both kinds of materials. Profilometric measurements were used to verify that the newly-introduced method is almost nondestructive for the investigated metals. The results obtained in the present work confirmed the potential of using this original LIBS system not only for the fast elemental analysis but also for the direct estimation of the hardness of metals and alloys. © 2020, Springer Science+Business Media, LLC, part of Springer Nature.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Ion temperature evolution in an ultracold neutral plasma

We study the long-time evolution of the ion temperature in an expanding ultracold neutral plasma using spatially resolved, laser-induced-fluorescence spectroscopy. Adiabatic cooling reduces the ion temperature by an order of magnitude during the plasma expansion, to temperatures as low as 0.2 K. Cooling is limited by heat exchange between ions and the much hotter electrons. We also present evidence for an additional heating mechanism and discuss possible sources. Data are described by a model of the plasma evolution, including the effects of ion-electron heat exchange. We show that for appropriate initial conditions, the degree of Coulomb coupling of ions in the plasma increases during expansion.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗
DOE OSTI2010

Dynamic Ionization of Water under Extreme Conditions

Raman spectroscopy in a laser heated diamond anvil cell and first principles molecular dynamics simulations have been used to study water in the temperature range 300 to 1500 K and at pressures to 56 GPa. We find a substantial decrease in the intensity of the O-H stretch mode in the liquid phase with pressure, and a change in slope of the melting line at 47 GPa and 1000 K. Consistent with these observations, theoretical calculations show that water beyond 50 GPa is 'dynamically ionized' in that it consists of very short-lived (<10 fs) H{sub 2}O, H{sub 3}O{sup +}, and OH{sup -} species, and also that the mobility of the oxygen ions decreases abruptly with pressure, while hydrogen ions remain very mobile. We suggest that this regime corresponds to a superionic state.

74 ATOMIC AND MOLECULAR PHYSICS↗
NASA NTRS2014

Volume Measurements of Laser-generated Pits for In Situ Geochronology using KArLE (Potassium-Argon Laser Experiment)

The Potassium-Argon Laser Experiment( KArLE), is composed of two main instruments: a spectrometer as part of the Laser-Induced Breakdown Spectroscopy (LIBS) method and a Mass Spectrometer (MS). The LIBS laser ablates a sample and creates a plasma cloud, generating a pit in the sample. The LIBS plasma is measured for K abundance in weight percent and the released gas is measured using the MS, which calculates Ar abundance in mols. To relate the K and Ar measurements, total mass of the ablated sample is needed but can be difficult to directly measure. Instead, density and volume are used to calculate mass, where density is calculated based on the elemental composition of the rock (from the emission spectrum) and volume is determined by pit morphology. This study aims to reduce the uncertainty for KArLE by analyzing pit volume relationships in several analog materials and comparing methods of pit volume measurements and their associated uncertainties.

French, R. A.↗
DOE OSTI2011

The CH2 b~1B1 - a~1 A1 Band Origin at 1.20 um

The origin band in the {tilde b}{sup 1}B{sub 1}-{tilde a}{sup 1}A{sub 1} transition of CH{sub 2} near 1.2 {mu}m has been recorded at Doppler-limited resolution using diode laser transient absorption spectroscopy. The assignments of rotational transitions terminating in upper state levels with K{sub a} = 0 and 1, were confirmed by ground state combination differences and extensive optical-optical double resonance experiments. The assigned lines are embedded in a surprisingly dense spectral region, which includes a strong hot band, {tilde b}(0,1,0) K{sub a} = 0 - {tilde a}(0,1,0) K{sub a} = 1 sub-band lines, with combination or overtone transitions in the {tilde a}{sup 1}A{sub 1} state likely responsible for the majority of unassigned transitions in this region. From measured line intensities and an estimate of the concentration of CH{sub 2} in the sample, we find the transition moment square for the 000 {l_arrow} 110 transition in the {tilde b}{sup 1}B{sub 1}(0,0,0)0-{tilde a}{sup 1}A{sub 1}(0,0,0)1 sub-band is 0.005(1) D{sup 2}. Prominent {tilde b}{sup 1}B{sub 1}(0,1,0)0-{tilde a}{sup 1}A{sub 1}(0,1,0)1 hot band lines were observed in the same spectral region. Comparison of the intensities of corresponding rotational transitions in the two bands suggests the hot band has an intrinsic strength approximately 28 times larger than the origin band. Perturbations of the excited state K{sub a} = 0 and 1 levels are observed and discussed. The new measurements will lead to improved future theoretical modeling and calculations of the Renner-Teller effect between the {tilde a} and {tilde b} states in CH{sub 2}.

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

SuperCam One Step Closer to Mars

The SuperCam instrument -- designed, built and tested at Los Alamos National Laboratory in partnership with the French Space Agency -- and destined for the exploration of Mars has completed testing and evaluation at Los Alamos and is on its way to the Jet Propulsion Laboratory in California for full system integration. SuperCam will be one of two Los Alamos instruments on the next rover, called Mars 2020, an upgraded version of the current rover on Mars, Curiosity. SuperCam consists of a "mast unit" and "body unit, the mast unit, mounted on a mast on the exterior of the rover, is essentially a telescope with a laser, an extremely advanced version of Laser Induced Breakdown Spectroscopy, or LIBS, a technology invented at Los Alamos. The laser blasts a tiny portion of a geological formation, both rocks and soils on Mars, creating a plasma. The telescope then captures the spectra of the light emitted by the plasma. The body unit, mounted inside the body of the rover, is essentially a sophisticated spectrometer, and uses the light spectra to determine both the elemental and molecular composition of the sample, along with physical properties like hardness. Launch of the Mars 2020 mission is scheduled for late July, 2020, followed by the landing on Mars in February of 2021.

2020↗
DOE OSTI2013

The Influence of spot size on the expansion dynamics of nanosecond-laser-produced copper plasmas in atmosphere

Laser produced copper plasmas of different spot sizes in air were investigated using fast photography and optical emission spectroscopy (OES). The laser energy was 33 mJ. There were dramatic changes in the plasma plume expansion into the ambient air when spot sizes changed from {approx}0.1 mm to {approx}0.6 mm. A stream-like structure and a hemispherical structure were, respectively, observed. It appeared that the same spot size resulted in similar expansion dynamics no matter whether the target was located in the front of or behind the focal point, although laser-induced air breakdown sometimes occurred in the latter case. Plasma plume front positions agree well with the classic blast wave model for the large spot-size cases, while an unexpected stagnation of {approx}80 ns occurred after the laser pulse ends for the small spot size cases. This stagnation can be understood in terms of the evolution of enhanced plasma shielding effects near the plasma front. Axial distributions of plasma components by OES revealed a good confinement effect. Electron number densities were estimated and interpreted using the recorded Intensified Charge Coupled Device (ICCD) images.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗
DOE OSTI2020

Effect of initial γ -irradiation on infrared laser ablation of poly(vinyl alcohol) studied by infrared spectroscopy

We report the effect of initial γ-irradiation of poly(vinyl alcohol) (PVA) on the kinetics of polymer ablation under CO 2 laser irradiation was studied using infra-red spectroscopy. The rate of laser ablation rapidly decreases with increasing time of laser ablation up to 10 s. Initial γ-irradiation of a dose up to 100 kGy reduces the rate of the laser ablation, just like the effect of laser exposure. The number of OH and CH groups decrease in PVA both with laser irradiation and with γ-irradiation. The number of OH groups decreases more under laser irradiation. Unsaturated bonds are formed in γ–irradiated PVA on the surface of the crater formed by laser ablation of the polymer that has undergone radiolysis. Increasing the dose of initial γ-irradiation from 100 to 2300 kGy leads to an increase in the intensity of the IR bands of the unsaturated bonds. The number of IR bands in the spectra of the laser ablation crater of PVA does not change with the dose of initial γ-irradiation. A dose of radiolysis of 3500 kGy significantly changes the IR spectra of both the ablation crater and the coating formed from the ablation products. Many bands characteristic for PVA are no longer present and the intensities of bands corresponding to unsaturated bonds are increased. A computational model for loss of water and ketone formation was developed for PVA and PVA including a diol using G3(MP2). The highest activation energy barrier step in the decomposition reaction was formation of the enol species and water was shown to catalyze all decomposition steps.

36 MATERIALS SCIENCE↗