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DOE OSTI2025

ElementLIBS User's Guide: An operational aid for use and development

Laser-Induced Breakdown Spectroscopy or LIBS is a rapid, in-situ analytical technique where a laser of known energy is pulsed at the surface of an analyte. The laser pulse rapidly heats a localized area to many thousand degrees Kelvin, ablating part of the analyte and turning it into a plasma. As the plasma cools, excited atoms return to a ground state with known emission energies. This emitted energy is captured by various spectrometers and provides a spectrum of the emitted energies and intensities. This spectrum can be analyzed to provide the elemental composition of a sample by using known emission lines and relative abundance. ElementLIBS was developed for the SciAps hand-held LIBS model Z300 but will work with any model that provides a LIBS spectrum of similar resolution. The Z300 has an integrated resolution of 1/30 nm with a range of approximately 180nm – 960nm, providing an output spectrum of 23431 pixels across three spectrometers. These criteria are only provided as a reference, as the software was designed to work with any size spectrum, provided the input file is of the correct format and the models were developed using the same framework. If spectra of varying dimensions are used, the software will fail without warning and unusual events could occur.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2025

Enhanced sensitivity for electron affinity measurements of rare elements

The electron affinity (EA), the energy released when a neutral atom binds an additional electron, is a fundamental property of atoms that is governed by electron-electron correlations and is strongly related to an element’s chemical reactivity. However, conventional techniques for EA determination lack the experimental sensitivity to probe very scarce samples. As a result, the EA for the heaviest elements of the periodic table is entirely uncharted. Here, we present a novel technique to determine EAs through Laser Photodetachment Threshold Spectroscopy, performed in an electrostatic ion beam trap to increase the samples’ exposure to laser photons and, thus, improve the experimental signal sensitivity by three orders of magnitude. Moreover, the additional exposure time allows the use of lower-power continuous-wave narrow-band lasers that reduce uncertainties associated with broadening effects induced by the laser bandwidth. By applying this technique, we measure the EA of 35 Cl to be 3.612720(44) eV, achieving state-of-the-art precision while employing five orders of magnitude fewer anions. The demonstrated sensitivity paves the way for systematic EA measurements across isotopic chains - including isotope shifts and hyperfine splittings - and ultimately for the first direct determination of electron affinities in superheavy elements.

Maier, F. M. [Univ. of Greifswald (Germany); Europ↗

DOE OSTI2020

The Effect of Intensity Fluctuations on Sequential X-ray Photon Correlation Spectroscopy at the X-ray Free Electron Laser Facilities

How materials evolve at thermal equilibrium and under external excitations at small length and time scales is crucial to the understanding and control of material properties. X-ray photon correlation spectroscopy (XPCS) at X-ray free electron laser (XFEL) facilities can in principle capture dynamics of materials that are substantially faster than a millisecond. However, the analysis and interpretation of XPCS data is hindered by the strongly fluctuating X-ray intensity from XFELs. Here we examine the impact of pulse-to-pulse intensity fluctuations on sequential XPCS analysis. We show that the conventional XPCS analysis can still faithfully capture the characteristic time scales, but with substantial decrease in the signal-to-noise ratio of the g2 function and increase in the uncertainties of the extracted time constants. We also demonstrate protocols for improving the signal-to-noise ratio and reducing the uncertainties.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Spectral emission characteristics near 646 nm and plasma properties of laser-induced plasma of gaseous uranium hexafluoride

We present a detailed investigation of the temporal evolution of line and continuum emissions in laser-induced breakdown spectroscopy (LIBS) of gaseous uranium hexafluoride (UF 6 ), focusing on the spectral region near 646 nm. Spectral emission features, signal-to-background ratios (SBRs) of selected uranium lines, and spectral linewidths were examined under varying UF 6 pressures (15–60 Torr) and laser pulse energies (10–60 mJ). Higher pressures and pulse energies enhanced continuum emission and reduced SBRs but did not cause significant spectral congestion. Additional studies with the use of different laser systems, including nanosecond-pulsed Nd:YAG lasers (at fundamental and various harmonics) and a femtosecond-pulsed Ti:sapphire laser, revealed long-lived plasma continua in all cases. This persistent continuum is attributed to a pseudo-continuum from overlapping molecular emissions, as its intensity scales linearly with electron number density, deviating from the expected quadratic dependence of classical ion–electron interactions for free-free and free-bound continuum emission. Based on plasma persistence time, SBR, U II/U I intensity ratios, and electronic excitation temperature, no fundamental advantage was found for femtosecond-pulsed lasers over conventional nanosecond-pulsed ones for UF 6 enrichment assay with direct LIBS measurement.

Laser-induced breakdown spectroscopy↗

DOE OSTI2026

Ultrafast Laser Welding and Terahertz Time-domain Spectroscopy of Soda Lime Silicate Glass

Joining and welding techniques of similar and dissimilar materials have reached their limits due to the inflexibility of adapting dielectric materials, e.g., glasses and ceramics, reproducibility for transparent materials, and cycle process time. The ability to join pieces of glasses using laser irradiation allows rapid processing of vacuum insulating glass (VIG) for a widening range of commercial energy-efficient applications. We have used a 1064-nm laser wavelength with 15 picoseconds pulse width and a 155-kHz repetition rate to weld commercial plate glass pieces. The welded samples were characterized via x-ray fluorescence (XRF), time-of-flight secondary ion mass spectrometry (TOF–SIMS), polarimetry, and terahertz time-domain spectroscopy (THz-TDS) to determine the integrity of the weld and chemical changes in the welded areas. Our data shows no significant changes in glass chemistry and structure on average over nano- to micro-scales occurred from the welding process within the limits of the characterization tools. Our results demonstrate successful welding of glass plates without significant changes in the glass chemistry, structure, or properties in the laser-modified region or strains in the bulk glass.

Matthies, Kathleen [ORNL] (ORCID:0009000213135441)↗

DOE OSTI2025

Comparison of atomized mass and crater volume in laser ablation

The extent and dynamics of laser ablation are typically studied using crater imaging or by invoking the relationship between atomic emission and the mass removed. The former is a static view of a dynamic process and requires the accumulation of multiple shots in one location. The latter is complex and not absolute without calibration of the optical system with a standard of spectral radiance. We measure the mass of the atomized plume by laser atomic-absorption spectroscopy at 2 µs without external mass calibration; mass uncertainty in laser-ablation atomic absorption spectroscopy (LA-AAS) results from uncertainties in line area fitting, tabulated oscillator strengths, and partition functions as well as a <10% underrepresentation of the mass due to treating the plasma as a single thermodynamic equilibrium. The LA-AAS-measured mass pertains to the atoms in the probed charge states and does not include condensed or molecular species. The ablation efficiency at 300 mbar of helium varies significantly between the two focusing conditions used. A comparison of crater-derived masses and LA-AAS masses suggests that more defocused ablation may result in significant redeposition of material in the crater, distorting the conclusions from drilling studies and crater imaging. More focused ablation conditions result in crater-derived masses that exceed those measured with LA-AAS and suggest melt expulsion or phase explosion.

Merten, Jonathan [Arkansas State University, Jones↗

DOE OSTI2022

Methods for multiphase laser ablation analysis

Methods of liquid and solid materials analysis by laser induced ablation spectroscopy are disclosed. The liquid and solid materials are analyzed in an instrument having one pulsed laser to produce emissive plasma plumes and ablate solid material. Liquid phase samples are aerosolized before streaming to an analysis zone where they are dissociated into a plasma plume. A large number of sites within solid phase sample structures and be analyzed using a movable x-y-z stage and displayed in a chemical map.

Bol'shakov, Alexander A.↗

DOE OSTI2021

Carrier-specific dynamics in 2H-MoTe2 observed by femtosecond soft x-ray absorption spectroscopy using an x-ray free-electron laser

Femtosecond carrier dynamics in layered 2H-MoTe2 semiconductor crystals have been investigated using soft x-ray transient absorption spectroscopy at the x-ray free-electron laser (XFEL) of the Pohang Accelerator Laboratory. Following above-bandgap optical excitation of 2H-MoTe2, the photoexcited hole distribution is directly probed via short-lived transitions from the Te 3d5/2 core level (M5-edge, 572–577 eV) to transiently unoccupied states in the valence band. The optically excited electrons are separately probed via the reduced absorption probability at the Te M5-edge involving partially occupied states of the conduction band. A 400 ± 110 fs delay is observed between this transient electron signal near the conduction band minimum compared to higher-lying states within the conduction band, which we assign to hot electron relaxation. Additionally, the transient absorption signals below and above the Te M5 edge, assigned to photoexcited holes and electrons, respectively, are observed to decay concomitantly on a 1–2 ps timescale, which is interpreted as electron–hole recombination. The present work provides a benchmark for applications of XFELs for soft x-ray absorption studies of carrier-specific dynamics in semiconductors, and future opportunities enabled by this method are discussed.

2D materials↗

DOE OSTI2024

Protocols for x-ray transient grating pump/optical probe experiments at x-ray free electron lasers

Abstract Transient grating spectroscopy is a specialized application of the four-wave-mixing methodology and constitutes a versatile technique for investigating the dynamics of vibrational, magnetic and electronic degrees of freedom of matter in a background-free fashion. Recent developments in free-electron laser sources have enabled the extension of this technique into the extreme ultraviolet range. Ongoing efforts to expand transient grating spectroscopy into the x-ray regime promise numerous advantages: (1) substantial penetration depths that allow for probing bulk material properties, (2) element specificity via specific core-excited states, and (3) short wavelengths that allow for excitation gratings with higher momentum transfer and improved spatial resolution. In this study, we comprehensively outline the procedures for conducting x-ray transient grating pump/optical probe experiment. The process encompasses the design and alignment of the experimental setup, as well as the subsequent steps involved in data acquisition and analysis. This paper is intended as a comprehensive guide for researchers interested in implementing x-ray transient grating spectroscopy, providing valuable insights into the intricacies of the experimental workflow required for this novel technique. Furthermore, we discuss the potential for extending this methodology to an x-ray pump/x-ray probe scheme, envisioning a future direction that holds promise for enhancing the capabilities and scope of x-ray transient grating spectroscopy, opening new opportunities for studying ultrafast processes with unprecedented temporal and spatial resolutions.

Optics↗

DOE OSTI2023

Implementing an electronic sideband offset lock for isotope shift spectroscopy in radium

We demonstrate laser frequency stabilization with at least 6 GHz of offset tunability using an in-phase/quadrature (IQ) modulator to generate electronic sidebands (ESB) on a titanium sapphire laser at 714 nm and we apply this technique to perform isotope shift spectroscopy of 226 Ra and 225 Ra. By locking the laser to a single resonance of a high finesse optical cavity and adjusting the lock offset, we determine the frequency difference between the magneto-optical trap (MOT) transitions in the two isotopes to be 2630.0 ± 0.3 MHz, a factor of 29 more precise than the previously available data. Using the known value of the hyperfine splitting of the 3 P 1 level, we calculate the isotope shift for the 1 S 0 to 3 P 1 transition to be 2267.0 ± 2.2 MHz, a factor of 8 more precise than the best available value. Our technique could be applied to countless other atomic systems to provide unprecedented precision in isotope shift spectroscopy and other relative frequency comparisons.

47 OTHER INSTRUMENTATION↗

DOE OSTI2024

Wavelength modulation laser-induced fluorescence for plasma characterization

Laser-Induced Fluorescence (LIF) spectroscopy is an essential tool for probing ion and atom velocity distribution functions (VDFs) in complex plasmas. VDFs carry information about the kinetic properties of species that is critical for plasma characterization. Accurate interpretation of these functions is challenging due to factors such as multicomponent distributions, broadening effects, and background emissions. Our research investigates the use of Wavelength Modulation (WM) LIF to enhance the sensitivity of VDF measurements. Unlike standard Amplitude Modulation (AM) methods, WM–LIF measures the derivative of the LIF signal. This approach makes variations in VDF shape more pronounced. VDF measurements with WM–LIF were investigated with both numerical modeling and experimental measurements. The developed model enables the generation of both WM and AM signals, facilitating comparative analysis of fitting outcomes. Experiments were conducted in a weakly collisional argon plasma with magnetized electrons and non-magnetized ions. Measurements of the argon ion VDFs employed a narrow-band tunable diode laser, which scanned the 4p 4 D 7/2 –3d 4 F 9/2 transition centered at 664.553 nm in vacuum. A lock-in amplifier detected the second harmonic WM signal, which was generated by modulating the laser wavelength with an externally controlled piezo-driven mirror of the diode laser. Finally, our findings indicate that the WM–LIF signal is more sensitive to fitting parameters, allowing for better identification of VDF parameters such as the number of distribution components, their temperatures, and velocities. In addition, WM–LIF can serve as an independent method to verify AM measurements and is particularly beneficial in environments with substantial light noise or background emissions, such as those involving thermionic cathodes and reflective surfaces.

47 OTHER INSTRUMENTATION↗

DOE OSTI2024

Laser-Induced Plasmas of Plutonium Dioxide in a Double-Walled Cell

Plutonium research has been stifled by the significant number of administrative controls and safety procedures, space and instrumentation limitations in radiological gloveboxes, and the potential for personnel and equipment contamination. To address the limited number of spectroscopic studies in Pu-bearing compounds in the current scientific literature, this work presents the use of double-walled cells (DWCs) in “clean” buildings/laboratories as an alternative to research in radiological gloveboxes. This study reports the first laser-induced breakdown spectroscopy (LIBS) experiments of a PuO 2 pellet contained within a DWC, where the formation of elemental (atomic and ionic) species as well as the evolution from elemental to molecular products (Pu x O y ) was measured. Raman spectroscopy was also used to characterize the surface of the ablated pellet and the particulates deposited on the window of the inner cell. The full width half-maximum of the T 2g band enabled us to obtain an estimate of the temperature at the pellet surface after the ablation pulse and the particulates based on the crystal lattice disorder. Particulates deposited on the window of the DWC during laser ablation were characterized using scanning electron microscopy, where molten irregular particulates and spheroids were observed. This exciting research conducted in a DWC describes our initial attempts to incorporate LIBS in the arsenal of spectroscopic tools for nuclear forensics applications.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

DOE OSTI2025

The effect on soot and its gas precursors of doping ethylene with 2,2,4,6,6-pentamethyl-heptane in the nitrogen-fuel stream of a laminar non-premixed Planar Mixing Layer Flame (PMLF)

Synthetic Aviation Turbine Fuels (SATFs) are promising for reducing soot emissions from the aviation sector and diversifying Jet Fuel (JF) sources. Accurately predicting the combustion and emissions behavior of SATFs (and other JFs) necessitates robust experimental databases to elucidate the chemistry of long-chain iso-paraffins, which can compose up to two-thirds of SATF blends and whose behavior is considered to be well-represented by that of iso-dodecane isomers. Here, this study characterizes two laminar non-premixed Planar Mixing Layer Flames (PMLFs) with mild soot loads fueled by nitrogen-diluted ethylene, pure and doped with 2,2,4,6,6-pentamethyl-heptane, respectively. The two PMLFs have the same stoichiometric mixture fraction and total hydrocarbon mole fraction in the fuel stream (X F,F =X C2H4,F +X C12H26,F = 0.260), resulting in nearly the same maximum temperature (T max ≈1800 K) and simple identification of the effects of doping. Importantly, any horizontal PMLF cross-section has a self-similar structure that can be modeled as an equivalent One-Dimensional Counterflow Flame (1D-CF) with vanishingly small strain rate (a). The cross-section at a Height Above the Burner (HAB) of 50 mm is characterized in terms of C 0 -C 18 gas species using capillary sampling followed by GC-MS analyses. Laser-Induced Emission Spectroscopy (LIES) quantifies the soot volume fraction (ƒ v ) profiles at HAB=25 and 50 mm where Elastic Laser Light Scattering (E-LLS) is performed to determine the a of the equivalent 1D-CFs and the profile of the E-LLS equivalent diameter ( d 6,3 ) of soot. The substitution of 1500 ppm of ethylene with 2,2,4,6,6-pentamethyl-heptane causes an increase of ≈1.5 in the concentrations of several polycyclic aromatic hydrocarbons and fv. Concurrently, the measured d 6,3 doubles in the oxidizer stream, yet remains the same in the fuel stream, at HAB=50 mm. Instead, at HAB= 25 mm, the iso-dodecane doping does not affect the d 6,3 profile in either stream. The experimental results partially validate the chemical reactions and soot formation kinetic model developed at Lawrence Livermore National Laboratory and provide directions to further improve its predictions.

Iso-dodecane (2,2,4,6,6-Pentamethyl-Heptane)↗

DOE OSTI2025

Electronics Free Laser Sensing Technology for Minerals and Technology Elements

This presentation presents an electronics free laser sensing technique and its ongoing and potential applications. A laser-based technique, popularly known as laser-induced breakdown spectroscopy has been prototyped for the determination of high-tech elements including rare earth elements and other elements in solid as well as aqueous sources. All optical unit without any electronics has been designed in such a way that it can be installed in the source environment and connected to other required components for controlling and data acquisition from the workstation. Measurement methods and results obtained for selected elemental species and overall performance of the developed prototype will be presented.

HCM Sensor↗

DOE OSTI2026

Optimizing aluminum oxide passivation layers—Laser-induced plasmas for layer formation, real-time diagnostics, and layer evaluation

Molten salts have beneficial thermophysical and electrolytic properties, but the aggressive nature of molten salts requires corrosion mitigation strategies, such as structural material surface treatment. In this study, a laser-induced breakdown spectroscopy (LIBS) system was used to simultaneously ablate and monitor de-excitation spectra to form and identify dense alumina passivation layers. Additionally, high-frequency (kHz) LIBS imaging allowed rapid elemental mapping and depth profiling for surface O/Al ratios via minimally destructive analysis. The paired t-test rejected the null hypothesis that air and Ar cover gases were equivalent (p = 0.00012), and the analysis of variance (ANOVA) showed that overlap between shots (p = 0.03112) and cover gas flow rate (p = 0.02729) were statistically significant. At 75% overlap, the O/Al ratio increased to 10% ± 2%, and 90% overlap rose further to 31% ± 2%. Regardless of overlap, tuning the gas flow from 0.5 to 2.5 L min −1 enhanced the O/Al ratio by 24% ± 4%. LIBS depth profiling showed a 3× increase in layer thickness from 75% to 90% overlap. Molecular band peaks of AlO, a precursor to Al 2 O 3 found during treatment, suggest that band intensity could be used for real-time Al 2 O 3 optimization. Ultimately, by adjusting laser spot overlap and cover gas flow rate, a 266 nm laser was shown to form Al 2 O 3 layers on an Al6061 sample, with cover gas flow rate primarily affecting the O/Al ratio and layer thickness correlating with laser spot overlap. This combination of molecular spectra collection, imaging, and depth profiling demonstrated the robust layer analysis capabilities of LIBS.

Corrosion↗

DOE OSTI2026

SULI Report - Development of a Molten Salt Circulation Loop for in-situ Spectroscopy

This project supports the development of real time optical monitoring capabilities for molten salt reactor (MSR) environments by designing, testing, and refining a molten salt circulation loop suitable for combined laser induced breakdown spectroscopy (LIBS) and ultraviolet visible (UV Vis) absorption measurements. Online spectroscopic monitoring is increasingly important for nuclear safeguards, corrosion tracking, and material accountancy, yet MSR process fluids present substantial challenges due to their chemical complexity and hazards such as high temperatures and radiation. To address these needs, this work focuses on Phase I, the development of a room temperature aqueous circulation loop that serves as a surrogate platform for evaluating flow behavior, optical access, and component performance prior to high temperature salt operation. Initial testing identified several practical issues—including leaks, obstructions, and two-phase flow through the absorption cell—that were systematically resolved through hardware replacement, flow path redesign, and venturi pressure optimization. Relocating the flow cell upstream of the primary venturi enabled periods of stable single-phase flow, demonstrating the feasibility of integrating optical diagnostics into a circulation system. The results of Phase I provide essential design insight for Phase II, which will incorporate furnace compatible materials and LiCl KCl eutectic salt. Completion of the molten salt system will deliver a reusable testbed for evaluating multimodal spectroscopic techniques, advancing nondestructive, real time monitoring tools for future MSR and nuclear fuel cycle applications.

98 - NUCLEAR DISARMAMENT, SAFEGUARDS, AND PHYSICAL↗

DOE OSTI2026

Quantitative Analysis of Fission-Product Surrogates in Molten Salt Chloride Aerosols

This work demonstrates laser-induced breakdown spectroscopy (LIBS) applied to a stream of aerosolized salt from molten eutectic LiCl-KCl. We demonstrate analytical capabilities to track fission-product surrogates of Cs, Sr, Pr, and Nd simultaneously, with application to monitor salts in pyroprocessing schemes and molten salt reactors. This work demonstrates limits of detection using LIBS on the order of 100 μg/g, which proves potentially applicable to monitoring fission-product concentrations in pyroprocessing applications. Additionally, this work explores fundamental aspects of plasma temperature and plasma electron density of the aerosolized species during LIBS with a specific focus on potential non-uniform plasma conditions in the aerosol.

74 - ATOMIC AND MOLECULAR PHYSICS↗

DOE OSTI2025

Rapid characterization of MSW and RDF feedstocks for waste-to-energy process using LIBS and ML techniques

The heterogeneity in the composition of municipal solid wastes (MSW) poses significant challenges in the production of biofuel and bioproducts. This research aims to enhance the accuracy and efficiency of waste analysis and characterization by introducing a fast characterization approach for MSW-derived refuse-derived fuels (RDF) by combining Laser-Induced Breakdown Spectroscopy (LIBS) with advanced machine learning (ML) techniques. The approach combines data pre-processing of LIBS spectra of RDF, and the development of ML models trained on domain and theory-based spectral features for predicting process parameters. These models are adept at predicting key process parameters like High Heating Value (HHV), carbon content, and volatile matter. This approach can achieve an average RRMSE of 2.13% and R 2 of 0.98 or higher for all considered parameters on testing data. This work demonstrates significant potential for improving waste sorting, processing efficiency, and environmental compliance over traditional labor- and time-intensive laboratory waste analysis and characterization.

09 BIOMASS FUELS↗