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All sourcesNASA NTRSDOE OSTI
DOE OSTI2025

Optical emission spectroscopy and imaging of low-pressure N2 plasmas generated by intense fast-pulsed electron beams

An optical emission spectroscopic (OES) and imaging characterization is conducted on N2 plasmas generated by a 100 keV fast-pulsed electron beam. The electron beams are injected into an N2 gas filled volume with a current of 4.5 kA (300 A/cm2) and a 100 ns pulse width. The characterization is conducted at the pressures, 1 Torr and 0.1 Torr, corresponding to two distinct regimes that exhibit significantly different plasma dynamics. Beam impact ionization is shown to be a primary mechanism for producing low temperature plasmas at 1 Torr during beam output. After beam termination, ionization by an inductive electric field becomes the primary mechanism for plasma formation later in time for both pressures. OES and plasma imaging are used in this work as a diagnostic tool to track the distribution of electronic, vibrational, and rotational state transitions and ionized species. This is achieved with the use of a multi-resolution suite of spectrometers capable of acquiring time-resolved spectra. Vibrational and rotational bands of the N2 second positive system (C3Πu→B3Πg) and the N2+ first negative system (B2Σu+→X2Σg+) are identified in both regimes as well as N+ states exclusively in the lower pressure regime. Vibrational and rotational spectra are shown to track the evolution of the time-varying plasma current. Plasma imaging also reveals spatially nonuniform plasma emission at 0.1 Torr. A few hundred shots are recorded to fully characterize the emissions, and results are shown to be highly reproducible (≤±1% with 2σ confidence).

Kaiser, E. R. (ORCID:0000000336493938)↗
DOE OSTI2022

Major to trace element imaging and analysis of iron age glasses using stage scanning in the analytical dual beam microscope (tandem)

Dark and clear silicate glasses formed during an iron age vitrification event ≈ 1500 years ago at the Broborg hillfort near Uppsala, Sweden have been analyzed using a scanning electron microscope equipped with a micro-X-ray fluorescence (μXRF) spectrometer. Correlated µXRF and electron beam-induced energy dispersive spectrometry (EDS) X-ray maps were collected via stage-scanning at constant velocity. This coupled procedure represents a new approach for the cultural heritage community to conduct analytical studies of archaeometric specimens composed of metal, ceramic, or mixed inorganic/organic materials, where major and trace element compositions are registered in space for areas up to the centimeter-length scale at micrometer-scale resolution. Overview images were used to select areas for EDS beam scan maps correlated with multispectral cathodoluminescence (CL) imaging and co-located quantitative EDS and μXRF point analysis. Fe, Ca, Mg, Ti, P, Mn, Zr, Zn, and Y are enriched in the dark glass, while Si, Al, K, Na, Ba, Sr, Rb, and Ga are enriched in the clear glass. Unmelted material is comprised predominately of quartz (SiO 2 ) along with trace apatite (Ca 5 (PO 4 ) 3 [Cl,OH]) and zircon (ZrSiO 4 ). Multivariate statistical analysis was used to measure the area fractions of high variance components while lower variance components represented phase mixtures. Differences between calculated melt viscosities for the glass compositions are consistent with field and laboratory observations. Coupled large area EDS and μXRF imaging shows significant promise for informed selection of higher spatial resolution and higher sensitivity follow-up studies, e.g., those performed using synchrotron analysis.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Simple, compact, high-resolution monochromatic x-ray source for characterization of x-ray calorimeter arrays

X-ray calorimeters routinely achieve very high spectral resolution, typically a few eV full width at half maximum (FWHM). Measurements of calorimeter line shapes are usually dominated by the natural linewidth of most laboratory calibration sources. This compounds the data acquisition time necessary to statistically sample the instrumental line broadening and can add systematic uncertainty if the intrinsic line shape of the source is not well known. To address these issues, we have built a simple, compact monochromatic x-ray source using channel cut crystals. A commercial x-ray tube illuminates a pair of channel cut crystals that are aligned in a dispersive configuration to select the Kα1 line of the x-ray tube anode material. The entire device, including the x-ray tube, can be easily hand-carried by one person and may be positioned manually or using a mechanical translation stage. The output monochromatic beam provides a collimated image of the anode spot with magnification of unity in the dispersion direction (typically 100 μm–200 μm for the x-ray tubes used here) and is unfocused in the cross-dispersion direction so that the source image in the detector plane appears as a line. We measured output count rates as high as 10 count/s/pixel for the Hitomi soft x-ray spectrometer, which had 819 μm square pixels. We implemented different monochromator designs for energies of 5.4 keV (one design) and 8.0 keV (two designs), which have effective theoretical FWHM energy resolution of 0.125 eV, 0.197 eV, and 0.086 eV, respectively; these are well-suited for optimal calibration measurements of state-of-the art x-ray calorimeters. We measured an upper limit for the energy resolution of our Cr Kα1 monochromator of 0.7 eV FWHM at 5.4 keV, consistent with the theoretical prediction of 0.125 eV.

47 OTHER INSTRUMENTATION↗
DOE OSTI2024

Investigating the effects of precise mass measurements of Ru and Pd isotopes on machine learning mass modeling

Atomic masses are a foundational quantity in our understanding of nuclear structure, astrophysics, and fundamental symmetries. The longstanding goal of creating a predictive global model for the binding energy of a nucleus remains a significant challenge, however, and prompts the need for precise measurements of atomic masses to serve as anchor points for model developments. We present precise mass measurements of neutron-rich Ru and Pd isotopes performed at the Californium Rare Isotope Breeder Upgrade facility at Argonne National Laboratory using the Canadian Penning Trap mass spectrometer. The masses of 108 Ru, 110 Ru, and 116 Pd were measured to a relative mass precision $\delta$⁢$m/m$ ≈ 10 -8 via the phase-imaging ion-cyclotron-resonance technique, and represent an improvement of approximately an order of magnitude over previous measurements. Further, these mass data were used in conjunction with the physically interpretable machine learning (PIML) model, which uses a mixture density neural network to model mass excesses via a mixture of Gaussian distributions. The effects of our new mass data on a Bayesian-updating of a PIML model are presented.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗
DOE OSTI2020

Site-level Foliar C, N, delta13C data from samples collected during field survey associated with NEON AOP survey, East River, CO 2018

Carbon (C) and nitrogen (N) weight percent concentrations were obtained from the bulk foliar samples collected across East River, Washington Gulch, Slate River, and Coal Creek watersheds in Gunnison, Colorado during the summer of 2018. These samples were collected from sun-lit leaves of meadow, shrub, and tree vegetation types within 72 hours of the National Ecological Observatory Network Airborne Observation Platform (NEON AOP) hyperspectral survey. These samples were dried and then run on an elemental analyzer coupled to a mass spectrometer for C and N concentrations and delta13C. The intention of these data were to provide ground truth data to develop foliar nutrient models across the imaging spectroscopy domain. Additional associated site metadata and vegetation fractional cover information can be found in the associated data releases (DOI: 10.15485/1618130). Here we provide site level C, N, and delta 13C data in the CN_Results_Foliar.csv. All of these samples were also registered with IGSN codes, and the details from that registration with metadata for the samples is included in foliar_sample_igsn_metadata.csv.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2025

Rapid spatial analysis of surrogate TRISO fuel particles using laser-induced breakdown spectroscopy image analysis

Laser-induced breakdown spectroscopy (LIBS) mapping enables rapid elemental and spatial analysis of solid samples. In this work, surrogate TRi-structural ISOtropic (TRISO) particles with various layers consisting of Zr, W, C, and Si were used to demonstrate the use of a new thickness measurement tool developed to analyze elemental images generated from LIBS maps. Zr particles with varying outer-layer thicknesses ranging from 16 to 32 μm were measured with scanning electron microscopy with energy dispersive spectroscopy (SEM-EDS) and LIBS with both a complementary metal-oxide-semiconductor (CMOS) detector and an intensified charged coupled device (ICCD) detector. LIBS maps of particles were completed using CMOS and ICCD spectrometers with effective spatial resolutions of 4 and 2 μm, respectively. The novel thickness measurement tool identified layer regions within a LIBS map and then identified the locations of the boundaries between these layers. The tool then generated up to 1000 random profiles stemming radially from the center region, which were used to measure the layer thickness/radius. This image analysis tool demonstrated LIBS's ability to provide values comparable with SEM-EDS (3.7% relative difference) along with a 95% reduction in measurement time. Furthermore, the precision of these measurements was on par with the SEM-EDS measurements at <15% relative standard deviation. Following the analysis of the Zr particles, W particles with increased complexity (e.g., five versus three layers) were analyzed using both the CMOS and ICCD spectrometers simultaneously. The spatial dimensions were extracted with an average relative difference of 2.7% and an average relative standard deviation of 9%.

Andrews, Hunter B. [Oak Ridge National Laboratory ↗
DOE OSTI2025

Laser-driven high-resolution MeV x-ray tomography

The need for high-resolution MeV x-ray tomography to observe the three-dimensional structure of dense, large-sized objects is rapidly increasing for the non-destructive evaluation of critical additively manufactured parts, national security, and other applications. We report a demonstration of high-resolution MeV computed tomography of a dense, large object with a laser-driven x-ray source. A record detector-limited MeV radiograph resolution of < 200 µm as determined with the Bennett approximation of the point spread function was achieved by irradiating millimeter-thick tungsten targets with 300 TW femtosecond laser pulses at a 0.5 Hz repetition rate. A tungsten alloy step wedge spectrometer indicates that the peak of the x-ray emission is between 1 and 2 MeV, with an endpoint energy of 19 MeV. To illustrate the radiographic imaging capability of the system, a tomographic reconstruction of a nickel superalloy turbine blade ( maximum $ρr$ = 139 g/cm 2 ) with sub-millimeter resolution was performed using 2160 individual radiographs. The small x-ray source size opens the prospect of extremely high-resolution tomographs of large, dense objects. This laser-driven approach has major advantages for non-destructive evaluation.

47 OTHER INSTRUMENTATION↗
DOE OSTI2020

Dynamical Packing in the Habitable Zone: The Case of Beta CVn

Uncovering the occurrence rate of terrestrial planets within the habitable zone (HZ) of their host stars has been a particular focus of exoplanetary science in recent years. The statistics of these occurrence rates have largely been derived from transiting planet discoveries, and have uncovered numerous HZ planets in compact systems around M-dwarf host stars. Here we explore the width of the HZ as a function of spectral type, and the dynamical constraints on the number of stable orbits within the HZ for a given star. We show that, although the Hill radius for a given planetary mass increases with larger semimajor axis, the width of the HZ for earlier-type stars allows for more terrestrial planets in the HZ than late-type stars. In general, dynamical constraints allow ∼6 HZ Earth-mass planets for stellar masses ≳0.7M {sub ⊙}, depending on the presence of farther out giant planets. As an example, we consider the case of Beta CVn, a nearby bright solar-type star. We present 20 yr of radial velocities (RV) from the Keck/High Resolution Echelle Spectrometer (HIRES) and Automated Planet Finder (APF) instruments and conduct an injection-recovery analysis of planetary signatures in the data. Our analysis of these RV data rule out planets more massive than Saturn within 10 au of the star. These system properties are used to calculate the potential dynamical packing of terrestrial planets in the HZ and show that such nearby stellar targets could be particularly lucrative for HZ planet detection by direct imaging exoplanet missions.

79 ASTRONOMY AND ASTROPHYSICS↗
DOE OSTI2021

Using neutrons and x rays to measure plasma conditions in a solid sphere of deuterated polyethylene compressed to densities of 35 g/cc at temperatures of 2 keV and pressures of 40 Gbar

This paper describes an experiment that shock compresses the center of a solid deuterated polyethylene sphere, CD 2 , to densities of 35 g/cc and temperatures of 2 keV with corresponding pressure of 40 Gbar. The design employs a strong spherically converging shock launched through a solid ball of material using a Hohlraum radiation drive. As the shock coalesces at the center it produces a hot spot that we characterize by measuring the x-ray self-emission and 2.45 MeV neutrons emitted. Two-dimensional images and time-resolved measurements of the x rays emitted determine the size and time duration of the hot spot, leading to an estimated 2k eV electron temperature. The neutron time of flight spectrometer measures an average ion temperature of 1.06 ± 0.15 keV and neutron yield of 7.0 (±0.5) × 10 9 DD neutrons. Our new distribution function tool enables us to create a forward model of the experimental data based on 1D radiation-hydrodynamic simulations, leading to a better understanding of the plasma conditions that produce the measured neutrons and x rays. Furthermore, our simulations indicate that the x rays are produced in a short-lived hot-dense core over tens of picoseconds, whereas the neutron emission continues for about 200 ps, as the hot core starts to expand, thereby leading to a lower mean temperature of the plasma during neutron production. This finding is in agreement with the experimental data, and we therefore conclude that the forward-modeling is a useful tool for inferring the conditions of the hot spot in a laser-driven implosion during burn.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗
DOE OSTI2022

O 2 based resonantly ionized photoemission thermometry analysis of supersonic flows

Characterization of the thermal gradients within supersonic and hypersonic flows is essential for understanding transition, turbulence, and aerodynamic heating. Developments in novel, impactful non-intrusive techniques are key for enabling flow characterizations of sufficient detail that provide experimental validation datasets for computational simulations. In this work, Resonantly Ionized Photoemission Thermometry (RIPT) signals are directly imaged using an ICCD camera to realize the techniques 1D measurement capability for the first time. The direct imaging scheme presented for oxygen-based RIPT (O 2 RIPT) uses the previously established calibration data to direct excite various resonant rotational peaks within the S-branch of the C 3 Π, ( v = 2) ← X 3 Σ( v ′ = 0) absorption band of O 2 . The efficient ionization of O 2 liberates electrons that induce electron avalanche ionization of local N 2 molecules generating N 2 + , which primarily deexcites via photoemissions of the first negative band of N 2 + ( B 2 Σ <#comment/> u + − <#comment/> X 2 Σ <#comment/> g + ) . When sufficient lasing energy is used, the ionization region and subsequent photoemission signal is achieved along a 1D line thus, if directly imaged can allow for gas temperature assignments along said line; demonstrated here of up to five centimeters in length. The temperature gradients present within the ensuing shock train of a supersonic under expanded free jet serves as a basis of characterization for this new RIPT imaging scheme. The O 2 RIPT results are extensively compared and validated against well-known and established techniques (i.e., CARS and CFD). The direct imaging capability fully realizes the technique’s fundamental potential and is expected to be the standard of implementation going forward. The direct imaging capability can play instrumental roles in future scientific studies that rely upon acute characterization of thermal gradients within a medium that cannot be easily resolved by a point. Furthermore, the removal of the spectrometer greatly reduces the cost, complexity, and optical alignment associated with prior RIPT measurements.

42 ENGINEERING↗
DOE OSTI2024

Novel Instrumentation for Advanced Quantum Chromodynamics Studies with Flavor Sensitivity

The true nature of ordinary matter has always fascinated humankind, whose imagination has been pointed to the right direction since the 5th century BC with the first known atomic theory by Leucippus and Democritus. They described the matter as formed by small, invisible, indivisible, and eternal particles: the atoms. A long investigation followed them, including contributions from several of history?s greatest philosophers and scientists. The progress led to the understanding that atoms have an internal structure consisting of a central nucleus composed of protons and neutrons, surrounded by a cloud of electrons. About 50 years ago, scientists discovered that nucleons also have an internal structure. Through the Deep Inelastic Scattering (DIS) experiments, on which a lepton is scattered off a nucleon, it was possible to access the distribution of partons inside the nucleon along the longitudinal direction defined by the hard-scale probe. It was a crucial step in developing Quantum Chromodynamics (QCD), currently the best theory describing the subatomic matter. Ultimately, DIS was recognized as a limited tool to investigate the nucleon structure because it is mainly sensitive to observables at the probe?s energy scale. In recent decades, theoretical developments have allowed defining soft-scale observables by measuring more complex processes. Reactions such as Semi-Inclusive Deep Inelastic Scattering (SIDIS) with single or di-hadron production, can provide information about the momentum of parton inside the nucleon. In particular, polarized SIDIS allows access to the Transverse-Momentum-Dependent (TMD) parton distributions describing the correlations of the quark and gluon degrees of freedom in transverse momentum and spin. This study can provide three-dimensional imaging of nucleon structure and inner dynamics, as long as the hadronic component in the final state can be measured. Identifying the species of the produced particles provides information on the quark flavor and assumes a crucial role in this context. The thesis describes the work carried out by the author in preparing novel instrumentation for particle identification in the final state of DIS experiments, to support modern analysis of the parton dynamics within the basic confined object (nucleon) with flavor sensitivity. The work has been focused on the CLAS12 spectrometer in operation at Jefferson Laboratory (JLab), Newport News, VA, USA, and the ePIC experiment in preparation for the future Electron-Ion Collider (EIC) at Brookhaven National Laboratory (BNL), Long Island, NY, USA. CLAS12 is a fixed-target experiment using a 12 GeV beam of polarized electrons scattering off polarized nuclear targets. In 2018 and 2022, two Ring Imaging Cherenkov (RICH) detector modules were installed to improve the ?±/K± separation in the high-momentum region (3÷8 GeV/c) of the experiment. The author contributed to the assembly, installation, and com- missioning of the second RICH module, to the efficiency studies of the first module, and to the first SIDIS analysis with high-momentum kaons identified by the RICH. These studies led to the observation of the first spin asymmetry with high-momentum kaons from the CLAS12 experiment, and an initial assessment of the systematic error associated with the hadron identification. ePIC will be the first experiment at the future EIC, the new collider designed to expand the frontiers of QCD. The author was involved in the development of the dual-radiator Ring Imaging Cherenkov (dRICH). This detector will interpolate the measurements of the Cherenkov angles of photons produced by relativistic particles crossing two different radiators to identify charged hadrons. The author contributed to the studies conducted with the dRICH prototype, developing the reconstruction and analysis software and simulations, characterizing the aerogel radiator samples, and being responsible for the tracking system used during the beam tests. The performance obtained by the prototype has been progressively improved and the results are now comparable with the expectation derived from the simulation and satisfy the requirements of the experiment. In Chapter 1, the SIDIS theory is briefly introduced, outlying the connection with the experimental measurement. Chapter 2 includes the description of the CLAS12 RICH, its assembly and installation, and the efficiency study. In Chapter 3, the analysis of the Beam-Spin Asymmetry associated with SIDIS kaons is described. Chapter 4 describes the contribution to the dRICH for EIC, starting from a description of the ePIC experiment and focusing on the studies performed for the dRICH prototype. The conclusions of this work are summarized at the end.

Vallarino, Simone↗
DOE OSTI2022

Measurement of the Deeply Virtual Compton Scattering Cross Section from the Proton at 10.6 GeV using the CLAS12 Detector

Deeply Virtual Compton Scattering (DVCS) is an exclusive process that produces a real photon when a lepton scatters from a quark inside a nucleon or a nucleus. Measurement of the DVCS cross section enables the study of the Generalized Parton Distributions (GPD), which plays a central role in understanding the QCD dynamics inside a hadron. Thus, the quark and gluon origin of the nucleon spin and mass can be probed and three-dimensional images of the target nucleon or nucleus can be realized. This thesis presents a cross section analysis of DVCS from the proton in the presence of its background, Bethe-Heitler (BH) process. The CEBAF Large Acceptance Spectrometer for operation at 12 GeV beam energy (CLAS12) collaboration has taken electron-proton scattering data in fall 2018 using a liquid hydrogen target and the 10.6 GeV polarized electron beam from the Continuous Electron Beam Accelerator Facility (CEBAF). The CLAS12 detector is a nearly hermetic fixed-target detector, located in Hall B, Jefferson Lab at Newport News, Virginia. The experimentally determined BH-DVCS cross section is in good agreement with a phenomenological-model based theoretical prediction. The kinematic dependence of the cross section is reported over a wide range. The short-term plan to utilize the results presented here for a thorough tomography study and the long-term plan for GPD studies at future facilities such as the Electron-Ion Collider (EIC) are discussed.

Lee, Sangbaek↗
DOE OSTI2024

Photoinitiated Reactions of Molecules and Radicals in Molecular Beams

The UV photochemistry of organic molecules is a fundamental process that governs reactions in the atmosphere, synthetic chemistry, processing of organic aerosols, and biological damage in living tissues. In many organic molecules, the ensuing evolution involves pathways that are in competition, giving rise to different products, isomerization, coupling to other electronic states, and secondary reactive collisions. Because photodissociation is usually fast (picoseconds to microseconds), these processes are far from equilibrium and are controlled by kinetic competition and dynamical forces. The work accomplished was focused primarily on the photochemistry of alpha-keto carboxylic acids, a group of acids produced from natural sources, which are implicated in aerosol formation and biological processes. In the atmosphere, they are destroyed mainly by solar radiation. Studying their photochemistry has been surprisingly difficult because of the complexity of their excited electronic states, and the effect of collisions and secondary reactions. The second project investigated the lifetime of excited electronic states of pyrazine and picoline and had both experimental and theoretical aspects. The work focused on a model molecule, pyruvic acid (PA), because it was hypothesized that it should be a good source of the unstable carbene, methylhydroxycarbene (MHC). PA has an internal hydrogen bond that controls the evolution of its decomposition. The decomposition was studied following excitation to two of its lowest excited states reached by laser irradiation at 351 and 193 nm. The photodissociation dynamics in the absence and presence of collisions was monitored and compared. Understanding the UV photochemistry requires the use of complementary experimental approaches. Two methods were enlisted, which together generated a comprehensive and detailed set of results: (i) The time-sliced velocity map imaging (SVMI) instrument at USC was exploited to determine kinetic energy release of fragments, fast dissociation timescales, and internal state distributions of fragments for which Resonance Enhanced Multiphoton Ionization (REMPI) schemes exist; and (ii) The multiplexed photoionization mass spectrometer (MPIMS) setup developed at the Sandia Combustion Research Facility was used for product discovery, achieved by exploiting tunable narrowband VUV radiation at the Advanced Light Source (ALS), and to follow in real time their subsequent unimolecular and bimolecular reactions. The experimental conditions ranged from collisionless molecular beams to study nascent products to flow reactors of variable pressures to study subsequent bimolecular reactions of the products. The goals stated above were successfully accomplished. By exciting PA to its lowest excited state, MHC was identified as the only primary product and its isomerization to vinylalcohol and acetaldehyde was directly observed in real time. Moreover, we reported the first bimolecular reaction of MHC, which was with acetaldehyde, and identified its reaction product. This paves the way for the study of other reactions of this important carbene intermediate. When excitation was carried out at 193 nm, which imparted much higher energy to PA, many more products were directly observed in real time, some deriving from three-body dissociation. Quantitative branching ratios and secondary reactions of radical products were also determined and analyzed. The studies of pyrazine and picoline focused on the second excited state of these molecules and showed (via ionization studies) that their excited states were very short lived (<100 fs) because of efficient couplings to lower electronic states via vibronic coupling. Theoretical work on modeling the absorption spectrum and decay mechanisms of the excited states are in progress in collaboration with theoreticians.

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

Beamline Spectroscopy of Integrated Circuits With Hard X-Ray Transition Edge Sensors at the Advanced Photon Source

At Argonne National Laboratory, we are developing hard X-ray (2 to 20 keV) Transition Edge Sensor (TES) arrays for beamline science. The significantly improved energy resolution provided by superconducting detectors compared to semiconductor-based energy-dispersive detectors, but with better collection efficiency than wavelength-dispersive instruments, will enable greatly improved X-ray emission and absorption spectroscopic measurements. Additionally, a prototype instrument with 24 microwave-frequency multiplexed pixels is now in testing at the Advanced Photon Source (APS) 1-BM beamline. Initial measurements show an energy resolution ten times better (150 eV compared to < 15 eV) than the silicon-drift detectors currently available to APS beamline users, and in particular demonstrate the ability to resolve closely-spaced emission lines in samples containing multiple transition metal elements, such as integrated circuits. Comparing fluorescence spectra of integrated circuits measured with our TESs at the beamline to those measured with silicon detectors, we find emission lines and elements largely hidden (e.g. Hf alongside Cu) from a semiconductor-based detector but well resolved by a TES. This directly shows the strengths of TES-based instruments in fluorescence mapping.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2026

DESI Strong Lens Foundry. III. Keck Spectroscopy for Strong Lenses Discovered Using Residual Neural Networks

We present spectroscopic data of strong lenses and their source galaxies using the Keck Near-Infrared Echellette Spectrometer (NIRES) and the Dark Energy Spectroscopic Instrument (DESI), providing redshifts necessary for nearly all strong-lensing applications with these systems, especially the extraction of physical parameters from lensing modeling. These strong lenses were found in the DESI Legacy Imaging Surveys using residual neural networks and followed up by our Hubble Space Telescope program, with all systems displaying unambiguous lensed arcs. With NIRES, we target eight lensed sources at redshifts difficult to measure in the optical range and determine the source redshifts for six, between z s = 1.675 and 3.332. DESI observed one of the remaining source redshifts, as well as an additional source redshift within the six systems. The two systems with nondetections by NIRES were observed for a considerably shorter 600 s at high airmass. Combining NIRES infrared spectroscopy with optical spectroscopy from our DESI Strong Lensing Secondary Target Program, these results provide the complete lens and source redshifts for six systems, a resource for refining automated strong lens searches in future deep- and wide-field imaging surveys and addressing a range of questions in astrophysics and cosmology.

Agarwal, Shrihan [University of Chicago, IL (Unite↗
DOE OSTI2020

Trace Chemical Detection Using Intercalated MXenes as a Signal Enhancing Substrate in Optical Probes

MXenes are 2D materials composed of layered transition metal nitrides or carbides. These materials are synthesized by HF exfoliation from MAX phases (Ti{sub 3}AlC{sub 2}). The 2D nanomaterial was synthesized by the removal of the 'A' element, resulting in a Mxene product (Ti{sub 3}C{sub 2}). MXenes have the general formula M{sub n+1}X{sub n}T{sub x}, where M is an early transition metal, X is Carbon and/or Nitrogen, and T accounts for surface terminated functional groups such as Fluoride, hydroxyl, and oxygen. These materials have very unique properties, similar to graphene, that allows them to be applied in a variety of trace detection techniques including surface-enhanced Raman spectroscopy (SERS). MXenes have also been demonstrated to selectively uptake uranyl ion, UO{sub 2}{sup 2+}. If this property can be combined with SERS or fluorescence detection, it may be possible to use MXenes as the basis for an alternative method to kinetic phosphorescence analysis (KPA) for trace uranyl measurements. Objectives: To confirm that MXene Nano materials are suitable substrates for SERS and sensor development by enhancing Raman signaling. To determine if certain MXene preparation methods yield materials that are more suitable for trace sensing methods. To determine uranyl uptake properties of these MXene materials and test them for analytical signals. Sample Preparation: Preparation of Ti{sub 3}C{sub 2}MXene (at FSU). MXenes were prepared by etching Al from Ti{sub 3}AlC{sub 2} (MAX phase)material. Two etching techniques yield different MXene products: LiF/HCl: Milder reaction, larger MXene flakes. HF: Harsher reaction, smaller flakes, larger layer separation. Products washed to remove etchant, vacuum filtered, and dried. Dried MXene flakes are air-stable. Film preparation for sensor testing (at SRNL): Suspend powder in diH{sub 2}O, purge with Ar, sonicate for 30 min. Centrifuge and collect supernate with suspended particles. Observed LiF-etched Mxene yielded a higher density of particles and darker collected solution. Drop-cast (4 ml) supernate onto slides and dried with Ar. For Rhodamine B (RhB) testing, drop-cast 4 ml drops onto Mxene spots and dried with Ar. Scanning Electron Microscopy conditions: 10 kV Beam energy, high vacuum; Working distance of 8 mm; beam penetration depth appx. 4 microns, beam spot size appx. 2 nanometers. Results: Detection of aluminum correlates with bright spots on image. Presence of aluminum shows that LiF/HCl etching was less thorough than HF etching. Trace Cl detection in LiF images suggests incomplete rinsing. HF has smaller feature size, more layer structure, and increased homogeneity, consistent with expectations. Macroscopic Raman spectroscopy measurements: 532 nm excitation, ∼50 mW with a ∼100 micron spot size (InPhotonics RPB probe). Kaiser Optical Holospec f/1.8 spectrometer with cooled (-60 deg.C) Andor iDus OE420 CCD. LiF 1x supernate showed good signal for trace measurements of Rhodamine B. HF and 1/4x LiF supernates showed little Mxene or Rhodamine B signal. Low deposition densities led to excess background signal from glass slides. For LiF film, response is linear with Rhodamine B concentration over range tested. Will retest with Raman microscope (∼1 micron spot size) to characterize SERS of more dilute LiF and HF etched Mxenes. Conclusions: The LiF etched material was more suitable for macroscopic SERS measurements because it was more concentrated, resulting in a thicker film than the HF etched Mxene and diluted LiF sample. However, the other materials may give greater SERS enhancements, which we hope to determine from measurements with the Raman microscope. From characterization with SEM we concluded that the HF etched Mxene is more uniform/homogenous and has smaller particle size than the LiF etched Mxene. There is still aluminum present in both samples indicating that etching wasn't complete, but the removal of the aluminum was more efficient in the HF method. Path Forward: Observe SERS with Raman microscopy, to obtain better signals for the more diluted samples and be able to compare enhancement effects for the different MXenes. Characterize uranyl sorption into MXene films and test Raman and fluorescence signals. Revisit the etching conditions to improve removal of aluminum. FSU and SRNL will continue to collaborate to create and characterize different Mxene materials and test their usefulness for sensor applications.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2023

Exploring Mission Design for Imaging Spectroscopy Retrievals for Land and Aquatic Ecosystems

The retrieval algorithms used for optical remote sensing satellite data to estimate Earth's geophysical properties have specific requirements for spatial resolution, temporal revisit, spectral range and resolution, and instrument signal-to-noise ratio (SNR) performance to meet biogeoscience objectives. Studies to estimate surface properties from hyperspectral data use a range of algorithms sensitive to various sources of spectroscopic uncertainty, which are in turn influenced by mission architecture choices. Retrieval algorithms vary across scientific fields and may be more or less sensitive to mission architecture choices that affect spectral, spatial, or temporal resolutions and spectrometer SNR. We used representative remote sensing algorithms across terrestrial and aquatic study domains to inform aspects of mission design that are most important for impacting accuracy in each scientific area. We simulated the propagation of uncertainties in the retrieval process including the effects of different instrument configuration choices. We found that retrieval accuracy and information content degrade consistently at >10 nm spectral resolution, >30 m spatial resolution, and >8-day revisit. In these studies, the noise reduction associated with lower spatial resolution improved accuracy vis à vis high spatial resolution measurements. The interplay between spatial resolution, temporal revisit, and SNR can be quantitatively assessed for imaging spectroscopy missions and used to identify key components of algorithm performance and mission observing criteria.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2024

2D IR Microscopy—Technology for Visualizing Chemical Dynamics in Heterogeneous Environments (Final Technical Report)

The primary focus of this project was the design, prototype, and demonstration of a 2D IR microscope. The start date of this project was July 15, 2016 and the project end date was July 14, 2022. In the early years of this project our team designed, prototyped, and completely integrated a homebuilt microscope head with our high-repetition rate 2D IR spectrometer. Once in place our research team focused on characterizing the 2D IR microscope and using it to investigate model systems relevant to energy technologies. As part of this process, we identified two initial chemical systems to use to further develop 2D IR imaging modalities. The first chemical system developed was a room temperature ionic liquid (RTIL) electrolyte system and the second chemical system was a mixture of carbonates and salts developed as a battery electrolyte system. The completion of this project resulted in the full characterization of chemical dynamics in a bulk RTIL system and the demonstration of 2D IR imaging across the RTIL cast as a microdroplet in silicon oil. In addition, we explored the liquid structures and dynamics of organic carbonate mixtures from the vantage point of the vibrational probe, methyl thiocyanate. By the end of the project, we had moved toward in-depth studies of the organic carbonate mixtures.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗