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At least 163 records · Page 9
All sourcesNASA NTRSDOE OSTI
DOE OSTI2025

Surface-enhanced stimulated Raman spectroscopy with squeezed photonic states

Recent advances in generating light in specific quantum states facilitate new sensing applications and enhance or revitalize established measurement and sensing techniques. Stimulated Raman spectroscopy (SRS), a measurement modality based on Raman scattering, could benefit from tuning the quantum properties of the pump and the Stokes lights or the properties of quantum states of the stimulating and excitation fields. Additionally, this modality could also benefit from field enhancement accompanied by plasmon excitation in the surface regions of metal nanoparticles. We present a theoretical investigation of stimulated Raman scattering involving squeezed states of light. The concept of surface- and quantum-enhanced stimulated Raman scattering is introduced. Furthermore, expressions for the respective SRS transition rates are derived, and their dependence on the quantum states of the optical field is discussed, with particular emphasis on the squeezing parameters characterizing these states. For cases involving surface enhancements, we also employ classical computational electrodynamics to guide our exploration of atomically large systems that support plasmon excitation.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2023

Magnetoelastic interactions in SrCu 2 (BO 3 ) 2 studied by Raman scattering experiments and first principles calculations

Dynamic and static crystal lattice properties of SrCu 2 (BO 3 ) 2 are studied by means of Raman scattering, magnetostriction, and thermal expansion measurements in magnetic fields to 45 T. Raman experiments versus temperature reveal that some phonon modes show an unusual behavior: their frequencies soften (modes at 200 and 450 cm –1 ) while others harden (modes at 385 and 478 cm –1 ) when decreasing the temperature below 15 K. Magneto-Raman experiments show that their field dependence correlates with their respective temperature dependencies; e.g., modes that are hardened with increasing temperature also harden with applied magnetic fields and modes that become softer with temperature also soften with applied fields. We use density functional theory to successfully model and compute the energies of these modes, classifying them into two types: pantograph (modes that soften when decreasing the temperature) and nonpantograph. We conclude that the former involves the modification of the intradimer exchange interaction J and the latter the interdimer J'. Lastly, dilatometry is used to correlate field-dependent Raman modes to the closing of the spin gap as well as fractional-magnetization stripe states M = 1/4 M s and M = 1/3 M s , where M s is the saturation magnetization.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
NASA NTRS2024

Raman spectroscopy of Ryugu particles and their extracted residues: Fluorescence background characteristics and similarities to CI chondrites

We present here an investigation of Ryugu particles recovered by the Hayabusa2 space mission and their extracted carbonaceous acid residues using Raman spectroscopy. Raman parameters of Ryugu intact grains and their acid residues are characterized by broad D (defect induced) and G (graphite) band widths, indicating the presence of polyaromatic carbonaceous matter with low thermal maturity. Raman spectra of Ryugu particles and CI (type 1) chondrites exhibit stronger laser-induced fluorescence backgrounds compared to Type 2 and Type 3 carbonaceous chondrites. The high fluorescence signatures and wide bandwidths of the D and G bands of Ryugu intact grains are similar to the Raman spectra observed in CI chondrites, reflecting the low structural order of their aromatic carbonaceous matter, and strengthening the link between Ryugu particles and CI chondrites. The high fluorescence background intensity of the Ryugu particles is due to multiple causes, but it is likely that the relative abundance of geometry-bearing macromolecular organic matter in total organic carbon contents makes a large contribution to the fluorescence intensities. Locally observed high fluorescence in the acid-extracted residues of Ryugu is due to nitrogen-bearing outlier phase. The high fluorescence signature is one consequence of the low degree of thermal maturity of the organic matter and supports evidence that the Ryugu particles have escaped significant parent body thermal metamorphism.

Ryugu particles↗
DOE OSTI2022

Nearly degenerate two-color impulsive coherent Raman hyperspectral imaging

Impulsive stimulated Raman scattering (ISRS) is a robust technique for studying low frequency (<300 cm –1 ) Raman vibrational modes, but ISRS has faced difficulty in translation to an imaging modality. A primary challenge is the separation of the pump and probe pulses. Here we introduce and demonstrate a simple strategy for ISRS spectroscopy and hyperspectral imaging that uses complementary steep edge spectral filters to separate the probe beam detection from the pump and enables simple ISRS microscopy with a single-color ultrafast laser source. ISRS spectra are obtained that span from the fingerprint region down to <50 cm –1 vibrational modes. Furthermore, hyperspectral imaging and polarization-dependent Raman spectra are also demonstrated.

47 OTHER INSTRUMENTATION↗
DOE OSTI2025

Characterization of PuO 2 With Visible and UV Raman Spectroscopy: Discrimination Between the Bulk, Surface, and an Intermediate Disordered Layer

Raman spectroscopy is an ideal tool in the characterization of materials including PuO 2 . The wavelength-dependent absorptivity of the material defines the light penetration depth and the relative Raman scattering contribution from the bulk and the surface. Here, the surface contribution to the total Raman scattering was investigated for PuO 2 calcined at various temperatures and recorded with laser wavelengths of 355, 325, and 244 nm. These experiments provided the first glimpse of the wavelength-dependent disappearance and emergence of new phonons and electronic bands from the PuO 2 surface layers. The first indication of the wavelength transition in the Raman spectra was the loss of the 2LO2 (overtone, ~1155 cm -1 ) band and the weakening intensity of the Г 1 → Γ 5 electronic band (~2135 cm -1 ) with the 355-nm excitation laser. The Γ 5 electronic band was barely visible with the 244-nm excitation. The electronic band located at ~1050 cm -1 , corresponding to the Г 1 → Γ 4 electronic transition was observed to dramatically increase in intensity while the Г 1 → Γ 3 electronic band (2640 cm -1 ) sharpened as the UV wavelength was increased in energy from the near- to deep-UV (355–325–244 nm). The FWHM of the T 2g band was found to vary with calcination temperature (450°C and 900°C) with the 325-nm laser and the 244-nm laser. The T 2g band attributes, the strong emergence of the Г 1 → Γ 4 electronic band, and the disappearance of the 2LO2 overtone acquired with the 244-nm excitation for the different calcination temperatures suggest a shallow penetration depth.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
DOE OSTI2021

Fast and Non-Destructive Determination of Water Content in Ionic Liquids at Varying Temperatures by Raman Spectroscopy and Multivariate Regression Analysis

Imidazolium acetate ionic liquids (ILs) have been utilized as promising solvents in many applications that involve varying water content and temperature. These experimental variables affect the anion-cation intermolecular interactions, which in turn influence the performance of the ILs in these applications. Here, this paper shows Raman spectroscopy can be used as an operando method to measure water content in IL solvents when simultaneous temperature changes may occur. The Raman spectra of 1-alkyl-3-methylimidazolium acetate ILs (alkyl chain length n = 2, 4, 6, 8) with varying water content (from 0.028 to 0.899 water mole fraction) and temperature (from 78.1 K to 423.1 K) were measured. Increasing the water content or decreasing the temperature of the tested ILs weakens the anion-cation intermolecular interactions. The water content of these ILs can be quantified even in conditions when the temperature is changing using Raman spectroscopy combined with multivariate regression analysis, including principal component regression (PCR), partial-least-squares regression (PLSR), and artificial neural networks (ANNs). The ANN model combined with partial-least-squares (PLS) achieves the highest prediction accuracy of water content in ILs at varying temperatures (RMSECV = 0.017, R 2 CV = 99.1%, RMSEP = 0.019, R 2 P = 98.8%, RPD = 8.93). Raman spectroscopy provides a potential fast non-destructive operando method to monitor the water content of ILs even in applications when the temperature may be simultaneously altered; this information can lead to the optimized use of these ILs in many applications.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2024

Angle-resolved polarized Raman study of layered b-As x P x-1 alloys: Identification of As-P vibrational modes

In this study, the polarization-resolved Raman spectra of b-As x P x-1 flakes with varying arsenic concentration (x = 0, 0.4, and 0.8) are systematically investigated. A clear polarization dependence is observed in the Raman intensity of all the P-P, As-P, and As-As modes and confirmed by the first-principles calculations. The observed angle-dependence can be related to the structure of the Raman tensors of each peak. In particular, the Raman intensities corresponding to As-P vibration modes are studied in detail. The out of plane As-P mode ($A$$^{1}_{g}$) is clearly identified, but the butterfly-shaped behavior observed in the polar plot around 350 cm -1 is interpreted as the combination of the two in-plane vibrations, one along the armchair and the other along the zigzag direction. This work allows unambiguous assignment of the $A$$^{1}_{g}$, B 2g , and $A$$^{2}_{g}$ modes of the As-P vibrational modes and the importance of the consideration of the superposition of the in-plane B 2g and $A$$^{2}_{g}$ modes. Such study can be utilized to further characterize the anisotropic structural properties and analyze the local distribution of the As and P in b-As x P x-1 alloys which will play key roles in electronic and optical properties. Furthermore, this methodology can be further extended to alloyed two-dimensional material systems with in-plane anisotropy in general.

2D materials↗
DOE OSTI2025

High-pressure Cr 3+ luminescence and Raman spectroscopy of a natural MgAl 2 O 4 spinel to ∼60 GPa

Cr 3+ luminescence and Raman spectroscopy of a natural spinel were collected up to ∼60 GPa at ambient temperature using a Ne or a 4:1 methanol-ethanol mixture as the pressure transmitting media. Here, in the Ne experiments above ∼40 GPa, and in the 4:1 methanol–ethanol experiments above ∼20 GPa, all luminescence emission lines shift non-linearly, and by 59 GPa the spectra are broadened and are significantly changed. The Raman modes shift smoothly to higher frequencies with pressure, with a slight change in slope above 40 GPa, with no kinks or discontinuities. By ∼60 GPa, only the most intense Eg mode remains resolvable, appearing broadened and reduced in intensity. The change in slope in the Raman modes and luminescence bands may be due to a change in the compression mechanism of spinel. When spinel was decompressed from 40 GPa all changes were fully reversible; however, when the samples were decompressed from 54 to 60 GPa in Ne and 59 GPa in 4:1 methanol-ethanol the spectra were irreversibly changed. The change in the luminescence spectra and the Raman spectra are likely due to a pressure induced disorder of the anions or partial amorphization between 40 and 60 GPa.

Cr3+↗
DOE OSTI2024

Raman spectroscopy of uranium nitride kernels

Uranium nitride is an advanced fuel candidate for a wide variety of advanced nuclear reactors. This work summarizes the first characterization of UN kernels by Raman spectroscopy. First-principles density functional theory calculations were performed to predict the Raman spectra of uranium sesquinitride (U 2 N 3 ), uranium dinitride (UN 2 ), uranium mononitride (UN), uranium monocarbide (UC), as well as U-N-C (UN 1-x C x ) and a U-N-C-O mixture. Further, a core–shell structure was identified by scanning electron microscopy and Raman spectroscopy imaging. A signal at ~500 cm -1 was identified on the periphery of the core-shell structure, possibly corresponding to U 2 N 3 and/or UN 2 . This signal broadens and shifts to 470 cm -1 because of the formation of UNC, UNCO or U 2 N 3+x structures. The culmination of this work demonstrates the feasibility of using Raman spectroscopy to identify variations in composition and phases in UN kernels.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Post-detonation fireball thermometry via femtosecond-picosecond coherent anti-Stokes Raman Scattering (CARS)

Accurate knowledge of post-detonation fireball temperatures is important for understanding device performance and for validation of numerical models. Such measurements are difficult to make even under controlled laboratory conditions. Here, temperature measurements were performed in the fireball of a commercial detonator (RP-80, Teledyne RISI). The explosion and fragments were contained in a plastic enclosure with glass windows for optical access. A hybrid femtosecond-picosecond (fs-ps) rotational coherent anti-Stokes Raman scattering (CARS) instrument was used to perform gas-phase thermometry along a one-dimensional measurement volume in a single laser shot. The 13-mm-thick windows on the explosive-containment housing introduced significant nonlinear chirp on the fs lasers pulses, which reduced the Raman excitation bandwidth and did not allow for efficient excitation of high-J Raman transitions populated at flame temperatures. To overcome this, distinct pump and Stokes pulses were used in conjunction with spectral focusing, achieved by varying the relative timing between the pump and Stokes pulses to preferentially excite Raman transitions relevant to flame thermometry. Light scattering from particulate matter and solid fragments was a significant challenge and was mitigated using a new polarization scheme to isolate the CARS signal. Fireball temperatures were measured 35–40 mm above the detonator, 12–25 mm radially outward from the detonator centerline, and at 18 and 28 µs after initiation. At these locations and times, significant mixing between the detonation products and ambient air had occurred thus increasing the nitrogen-based CARS thermometry signal. Initial measurements show a distribution of fireball temperatures in the range 300–2000 K with higher temperatures occurring 28 µs after detonation.

42 ENGINEERING↗
DOE OSTI2024

Beyond the Charge Transfer Mechanism for 2D Materials-Assisted Surface Enhanced Raman Scattering

Two-dimensional (2D) materials have been extensively implemented as surface-enhanced Raman scattering (SERS) substrates, enabling trace-molecule detection for broad applications. However, the accurate understanding of the mechanism remains elusive because most theoretical explanations are still phenomenological or qualitative based on simplified models and rough assumptions. To advance the development of 2D material-assisted SERS, it is vital to attain a comprehensive understanding of the enhancement mechanism and a quantitative assessment of the enhancement performance. Here, the microscopic chemical mechanism of 2D material-assisted SERS is quantitatively investigated. The frequency-dependent Raman scattering cross sections suggest that the 2D materials’ SERS performance is strongly dependent on the excitation wavelengths and the molecule types. By analysis of the microscopic Raman scattering processes, the comprehensive contributions of SERS can be revealed. Beyond the widely postulated charge transfer mechanisms, the quantitative results conclusively demonstrate that the resonant transitions within 2D materials alone are also capable of enhancing the molecular Raman scattering through the diffusive scattering of phonons. Furthermore, all of these scattering routines will interfere with each other and determine the final SERS performance. Our results not only provide a complete picture of the SERS mechanisms but also demonstrate a systematic and quantitative approach to theoretically understand, predict, and promote the 2D materials SERS toward analytical applications.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2020

Surface Enhanced Raman Scattering Selectivity in Proteins Arises from Electron Capture and Resonant Enhancement of Radical Species

Plasmon-enhanced Raman scattering is a powerful approach to detecting and characterizing proteins in live and dynamic biological systems. However, the selective detection/enhancement of specific residues as well as spectral diffusion and fluctuations have complicated the interpretation of enhanced Raman spectra and images of biological matter. In this paper, we therefore demonstrate that the amino acid tryptophan (Trp) can capture an electron from an excited plasmon, which generates a radical anion that is resonantly enhanced: a visible excited electronic state slides into resonance upon charging. This surface enhanced resonance Raman scattering (SERRS) mechanism explains the persistence of Trp signatures in the SERS and TERS spectra of proteins. Evidence for this picture includes the observation of visible resonances in the UV-Vis extinction spectrum, changes in the ground state vibrational spectrum, and plasmon-resonance dependent behavior. DFT calculations support the experimental observations. The behavior observed from the free Trp molecule is shown to explain the SERS spectrum of the Trp-cage protein. In effect, resonant Raman scattering from radicals formed through plasmonic excitation represents an under-investigated mechanism that may be exploited for chemical sensing applications. This work was supported by the National Institutes of Health Award R01-GM109988. The authors thank Hannah Shafaat for helpful discussions and providing an azurin sample for comparison. The authors also thank Joel Harris for providing constructive comments on our manuscript.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2025

Raman Fingerprints of Phase Transitions and Ferroic Couplings in van der Waals Multiferroic CuCrP 2 S 6

CuCrP 2 S 6 (CCPS), a type-II multiferroic material, exhibits unique phase transitions involving ferroelectric, antiferroelectric, and antiferromagnetic ordering. Here, in this study, we conduct a comprehensive investigation on the intricate phase transitions and their multiferroic couplings in CCPS across a wide temperature range from 4 to 345 K through Raman spectroscopic measurements down to 5 cm –1 . We first assign the observed Raman modes with the support of theoretical calculations and angle-resolved polarized Raman measurements. We further present clear signatures of phase transitions from the analyses of temperature-dependent Raman spectral parameters. Particularly, two low-frequency soft modes are observed at 36.1 cm –1 and 70.5 cm –1 below 145 K, indicating the antiferroelectric to quasi-antiferroelectric transition. Moreover, phonon mode hardening is observed when the temperature increases from 4 to 65 K, suggesting negative thermal expansion (NTE) and strong magnetoelastic coupling below 65 K. These findings advance the understanding of vdW multiferroic CCPS, paving the way for future design and engineering of multiferroicity in cutting-edge technologies, such as spintronics and quantum devices.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2025

Evidence for Ga clusters in β-Ga 2 O 3 from Raman spectroscopy and density functional theory

Monoclinic gallium oxide (β-Ga 2 O 3 ) single crystals have a Raman mode at ∼250 cm −1 that is strongly correlated with free-electron density. Prior work attributed this peak to an electronic excitation of a shallow donor impurity band. However, heavily n-type thin films grown by metalorganic chemical vapor deposition or molecular beam epitaxy do not have the peak. In the present work, an alternate model is proposed: the 250 cm −1 Raman peak arises from Ga clusters, defined as two or more Ga atoms that form Ga–Ga bonds. Raman mapping reveals variations in the frequency that are consistent with a distribution of cluster sizes. The intensity of the peak decreases as the temperature is raised, attributed to melting of the Ga clusters. First-principles calculations indicate that the 250 cm −1 mode is due to Ga–Ga bond-stretching vibrations. As the Fermi energy is raised, the formation of Ga–Ga dimers becomes energetically favorable, explaining the correlation between n-type conductivity and the appearance of the Raman peak.

36 MATERIALS SCIENCE↗
DOE OSTI2024

SnSe 2 thermal conductivity from optothermal Raman and Stokes/anti-Stokes thermometry

The optothermal Raman method is useful in determining the in-plane thermal conductivity of two-dimensional (2D) materials that are either suspended or supported on a substrate. We compare this method with the Stokes/anti-Stokes scattering thermometry method, which can play a role in both calibration of Raman peak positions as well as extraction of the local phonon temperature. This work demonstrates that the Stokes/anti-Stokes intensity ratio plays an important role in determining the in-plane thermal conductivity of 2D tin diselenide (SnSe 2 ) dry-transferred onto a polished copper (Cu) substrate. The statistically-averaged thermal conductivity of the 108 ± 24 nm-thick SnSe 2 yielded 5.4 ± 3.5 Wm −1 K −1 for the optothermal Raman method, and 2.40 ± 0.81 Wm −1 K −1 for the Stokes/anti-Stokes thermometry method, indicating that the Stokes/anti-Stokes thermometry method to calculate the thermal conductivity of a material can simultaneously increase both precision and accuracy. The uncertainty value was also lowered by a factor of 1.9 from the traditional optothermal Raman method to the Stokes/anti-Stokes thermometry method. The low in-plane thermal conductivity of 2D SnSe 2 , 1.3–2.9 times lower than bulk, is useful for applications in thermal and electrical energy conversion and thermoelectric devices.

2D materials↗
DOE OSTI2023

Determination of Thermal Damage Threshold in THz Photomixers Using Raman Spectroscopy

The increase of device lifetime and reliability of THz photomixers will play an essential role in their possible future application. Therefore, their optimal work conditions/operation range, i.e., the maximal incident optical power should be experimentally estimated. We fabricated and tested THz photomixer devices based on nitrogen-implanted GaAs integrated with a Bragg reflector. Raman spectroscopy was applied to investigate the material properties and to disclose any reversible or irreversible material changes. The results indicate that degradation effects in the photomixer structures/material could be avoided if the total optical power density does not exceed levels of about 0.7 mW/µm 2 for 100 min of operation. Furthermore, the investigations performed during 1000 min of optical exposure on the photomixer devices’ central region comprising interdigitated metal-semiconductor-metal (MSM) structures suggest a reversible “curing” mechanism if the power density level of ~0.58 mW/µm 2 is not exceeded. Long-term operation (up to 1000 h) reveals that the photomixer structures can withstand an average optical power density of up to ~0.4 mW/µm 2 without degradation when biased at 10 V. Besides the decrease of the position of the A1g (LO) Raman mode from ~291 cm -1 down to ~288 cm -1 with increasing optical power density and operation time, broad Raman modes evolve at about 210 cm -1 , which can be attributed to degradation effects in the active photomixer/MSM area. In addition, the performed carrier lifetime and photomixer experiments demonstrated that these structures generated continuous wave sub-THz radiation efficiently as long as their optimal work conditions/operation range were within the limits established by our Raman studies.

36 MATERIALS SCIENCE↗
NASA NTRS2021

Raman Temperature and Density Measurements in Supersonic Jets

Prediction of flow-field properties in supersonic jets using computational fluid dynamics (CFD) code predictions has become routine; however, obtaining accurate solutions becomes more challenging when there is a significant temperature difference between the jet core and the ambient air and/or compressibility effects are significant. Benchmark sets of flow field property data are required in order to assess current CFD capabilities and develop better modeling approaches for these turbulent flow fields where accurate calculation of temperatures and turbulent heat flux is important. Particle Image Velocimetry (PIV), spontaneous rotational Raman scattering (SRS) spectroscopy and Background Oriented Schlieren (BOS) have been previously used to acquire measurements of the mean and root mean square (rms) velocities, the mean and rms gas temperatures and density gradients in subsonic jet flows and film cooling flows. In this work, the ability to measure density is added to the list of measurands available using the acquired Raman spectra. The suite of measurement techniques are now applied to supersonic jet flows. The computation of the local gas pressure in the potential core of an over-expanded jet is demonstrated using the Raman measured gas temperature and density. Additionally, a unique density feature in temperature matched, perfectly expanded jet flow shear layers identified using BOS was verified using the Raman measurement technique. These non-intrusive flow measurements are compared against RANS predictions of the supersonic jet flow properties as a means of assessing their prediction accuracy.

Raman Spectroscopy↗
NASA NTRSDate not supplied

Algorithmic Classification of Raman Spectra Biosignatures: Improving Life Detection Confidence

“Agnostic” biosignatures – indicators of life (or the absence of life), independent of a particular biochemistry – are increasingly considered a high standard for life detection. The Ladder of Life Detection (2018) called for investigating how combinations of independent and different potential biosignatures affect confidence. To address this gap, statistical classification of elemental abundances, isotopic fractionation, and reflectance spectroscopy (VNIR) has been implemented. Raman spectroscopy, highly desirable due to its wide availability, has the potential to improve this predictive power. This work implemented biosignature classification algorithms on Raman data alone, in preparation for combination with the other data types. Raman spectroscopy data was collected from published databases and papers as part of a manually curated dataset of “indicative” and “non-indicative of life” samples. These currently include 61 non-indicative samples (meteorites, magnetite); 3 indicative living samples (bacteria); 20 indicative non-living samples (chalk, bone); and 12 indicative mixed (with non-indicative material) samples (soil, microbial mats). Laboratory work is ongoing to characterize additional samples, particularly a greater breadth of mixed systems. Spectra were interpolated, filtered with the Savitzsky-Golay filter, and de-noised. For a preliminary examination, agnostic features were manually extracted including mean intensity, number of peaks, and mean peak width. Different peak prominences and filtering polynomials were used to refine features. Classification algorithms were implemented: k-nearest neighbors (KNN), logistic regression (LR), linear support vector machines (SVM), random forest (RF), Gaussian naïve bayes (GNB). Lastly, Monte Carlo simulations on 1,000 50%-train-test-splits were used to validate classification performance and feature significance. The preliminary feature set achieved its highest AUC of 0.52 with LR, with no strongly discriminatory features. Work to improve feature extraction, such as through deep learning with back propagation, is planned. In future work, the Raman data will be combined with the other data types, and potentially new data types such as enantiomeric excess. This project was partially supported through the NASA Ames Project EXcellence (APEX) incubator program.

Astrobiology↗