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NASA NTRS1985

Reassessment of the theory of stimulated Raman scattering

A modification of the standard theory of stimulated Raman scattering (SRS) first proposed by Sparks (1974, 1975) is analyzed and shown to incorporate a possibly important physical effect; however, its original formulation is incorrect. The analysis is based on an exact numerical integration of the coupled equations of the modified theory, the results of which are compared with both the conventional theory of SRS and with one set of experimental data. A reformulation of the modified theory is suggested that leads to a gain which is in somewhat better agreement with the data than is the conventional theory.

Fralick, G. C.↗

NASA NTRS1989

Effects of core turbulence on jet excitability

The effects of varying freestream core turbulence on the evolution of a circular jet with and without tonal excitation are examined. Measurements are made on an 8.8 cm diameter jet at a Mach number of 0.3. The jet is excitated by plane waves at Strouhal number 0.5. For the excited and unexcited cases the turbulence level is varied by screens and grids placed upstream of the nozzle exit. The experiment results are compared with a theoretical model which incorporates a variable core turbulence and considers the energy interactions between the mean flow, the turbulence and the forced component. Both data and theory indicate that increasing the freestream turbulence diminishes the excitability of the jet and reduces the effect of excitation on the spreading rate of the jet.

Mankbadi, Reda R.↗

NASA NTRS1982

Rayleigh, Raman and particulate scattering

Analysis of the visible and near infrared spectra of planetary atmospheres and the multiple scattering of photons within the atmosphere are discussed. Photons detected within the spectral region are solar photons which were scattered by the gas and particles in the planetary atmosphere. An example is given for the incident and emitted fluxes for a hypothetical planet with an effective temperature of 100 K. The absorption spectrum of the planetary atmosphere is discussed in terms of the various scattering processes photons undergo within the atmosphere. Three different physical processes are considered. Rayleigh scattering and Raman scattering by the gas molecules, and scattering by any cloud or dust aerosol particles in the atmosphere. The physics of each of these processes is examined.

Cochran, W. D.↗

DOE OSTI2024

Spectroscopic Analysis of Pu-bearing Compounds in Double-Walled Cells

Spectroscopic analysis of radiological materials has been historically limited to radiological labs with 11 older or less advanced scientific instrumentation. The development of double-walled cells (DWCs) at 12 the Savannah River National Laboratory (SRNL) has enabled Pu-bearing compounds to be removed 13 from radiological laboratories and studied in our radiologically clean spectroscopy lab with state-of14 the-art instrumentation. In this manuscript, we discuss the contributions of DWCs that have allowed 15 the application of Raman spectroscopy, diffuse reflectance infrared Fourier transform spectroscopy 16 (DRIFTS), diffuse reflectance spectroscopy (DRS) in the shortwave infrared, and gamma 17 spectroscopy at SRNL. Significant advances have been made in the understanding of thermal 18 decomposition of Pu(III) and Pu(IV) oxalates, the alpha-induced damage to the PuO2 crystal lattice, 19 and the effect of calcination temperatures to the quality of PuO2. These techniques have enabled 20 methods to conduct PuO2 age dating since last calcination and estimate the calcination temperature 21 with Raman and DRS. Additional spectroscopic information measured with DRIFTS has provided a 22 path to observe the evolution of carbon species with calcination temperature while gamma 23 spectroscopy provides information on age dating since last purification.

Villa-Aleman, Eliel↗

NASA NTRS1987

Raman spectra of adsorbed layers on space shuttle and AOTV thermal protection system surface

Surfaces of interest to space vehicle heat shield design were struck by a 2 W argon ion laser line while subjected to supersonic arc jet flow conditions. Emission spectra were taken at 90 deg to the angle of laser incidence on the test object. Results showed possible weak Raman shifts which could not be directly tied to any particular parameter such as surface temperature or gas composition. The investigation must be considered exploratory in terms of findings. Many undesirable effects were found and corrected as the project progressed. For instance, initial spectra settings led to ghosts which were eliminated by closing the intermediate of filter slit of the Spex from 8 to 3 mm. Further, under certain conditions, plasma lines from the laser were observed. Several materials were also investigated at room temperature for Raman shifts. Results showed Raman shifts for RCC and TEOS coated materials. The HRSI materials showed only weak Raman shifts, however, substantial efforts were made in studying these materials. Baseline materials showed the technique to be sound. The original goal was to find a Raman shift for the High-temperature Reusable Surface Insulation (HRSI) Reaction Cured borosilicate Glass (RCG) coated material and tie the amplitude of this peak to Arc jet conditions. Weak Raman shifts may be present, however, time limitations prevented confirmation.

Willey, Ronald J.↗

DOE OSTI2024

Synthesis of hierarchical graphene coated porous Si anode for lithium-ion batteries

The ultra-high capacity and widespread availability of Si materials have resulted in them being the focus of extensive studies to replace the graphite anode. However, the main barriers preventing the Si anodes from large-scale applications are their huge volume change and severe interface reactions in the lithiation/delithiation process, which pulverizes its structure and subsequently deteriorates its cycle life. Here, micrometer-scale porous Si coated with graphene coating (mpSi@G) has been synthesized by using SiO 2 nanoparticles and novel coal-derived humic acid as feedstocks through a magnesiothermic reduction, followed by spray drying and calcination techniques. SEM, Raman, and X-ray absorption analysis demonstrate that the hierarchical graphene shell and micrometer-sized porous Si structure effectively release the Si anode's mechanical stress upon lithiation to achieve good structural stability. Here, the synthesized mpSi@G anode delivers a high initial lithiation capacity of 2974.9 mAh g –1 at 0.1 A g –1 with an initial coulombic efficiency of 70.2 %. Furthermore, the conductive hierarchical graphene network, along with the tight contacts of porous-Si and the graphene shell, contribute to a high capacity of 1109.5 mAh g –1 at a high current density of 5.0 A g –1 , showing excellent rate capability.

25 ENERGY STORAGE↗

DOE OSTI2024

Laser-induced graphene gas sensors for environmental monitoring

Artemesia tridentatais a foundational plant taxon in western North America and an important medicinal plant threatened by climate change. Low-cost fabrication of sensors is critical for developing large-area sensor networks for understanding and monitoring a range of environmental conditions. However, the availability of materials and manufacturing processes is still in the early stages, limiting the capacity to develop cost-effective sensors at a large scale. In this study, we demonstrate the fabrication of low-cost flexible sensors using laser-induced graphene (LIG); a graphitic material synthesized using a 450-nm wavelength bench top laser patterned onto polyimide substrates. We demonstrate the effect of the intensity and focus of the incident beam on the morphology and electrical properties of the synthesized material. Raman analyses of the synthesized LIG show a defect-rich graphene with a crystallite size in the tens of nanometers. This shows that the high level of disorder within the LIG structure, along with the porous nature of the material provide a good surface for gas adsorption. The initial characterization of the material has shown an analyte response represented by a change in resistance of up to 5% in the presence of volatile organic compounds (VOCs) that are emitted and detected byArtemisiaspecies. Bend testing up to 100 cycles provides evidence that these sensors will remain resilient when deployed across the landscapes to assess VOC signaling in plant communities. The versatile low-cost laser writing technique highlights the promise of low-cost and scalable fabrication of LIG sensors for gas sensor monitoring.

Chemistry↗

NASA NTRS1971

A study of transient stimulated Raman scattering and self-focusing in the picosecond time regime

Two third order processes, stimulated Raman scattering and self-focusing, with picosecond pulses are studied. In the case of transient stimulated scattering, the gain is reduced from the steady state value, and qualitatively new features, such as shortening and delay of the Stokes pulse relative to the laser pulse, appear. These predictions are extended to realistic laser pulses, and experiments confirm all of the theoretical predictions. The self-focusing and frequency broadening of picosecond pulses is studied in the absence of stimulated Raman scattering in several materials with large orientational Kerr constants. Measurements of the relaxation time indicate that the orientational Kerr effect is important in the self-focusing of picosecond pulses. Self-focused filaments are observed to propagate with constant diameters over a distance greater than 10 cm, but disappear before the end of a 20 cm cell. The filaments radiate light continuously along their path and the spectrum of the light shows that the frequency content extends symmetrically for several hundred wave numbers on either side of the laser frequency.

Reintjes, J. F.↗

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 NTRS2005

Improvement of Raman lidar algorithm for quantifying aerosol extinction

Aerosols are particles of different composition and origin and influence the formation of clouds which are important in atmospheric radiative balance. At the present there is high uncertainty on the effect of aerosols on climate and this is mainly due to the fact that aerosol presence in the atmosphere can be highly variable in space and time. Monitoring of the aerosols in the atmosphere is necessary to better understanding many of these uncertainties. A lidar (an instrument that uses light to detect the extent of atmospheric aerosol loading) can be particularly useful to monitor aerosols in the atmosphere since it is capable to record the scattered intensity as a function of altitude from molecules and aerosols. One lidar method (the Raman lidar) makes use of the different wavelength changes that occur when light interacts with the varying chemistry and structure of atmospheric aerosols. One quantity that is indicative of aerosol presence is the aerosol extinction which quantifies the amount of attenuation (removal of photons), due to scattering, that light undergoes when propagating in the atmosphere. It can be directly measured with a Raman lidar using the wavelength dependence of the received signal. In order to calculate aerosol extinction from Raman scattering data it is necessary to evaluate the rate of change (derivative) of a Raman signal with respect to altitude. Since derivatives are defined for continuous functions, they cannot be performed directly on the experimental data which are not continuous. The most popular technique to find the functional behavior of experimental data is the least-square fit. This procedure allows finding a polynomial function which better approximate the experimental data. The typical approach in the lidar community is to make an a priori assumption about the functional behavior of the data in order to calculate the derivative. It has been shown in previous work that the use of the chi-square technique to determine the most likely functional behavior of the data prior to actually calculating the derivative eliminates the need for making a priori assumptions. We note that the a priori choice of a model itself can lead to larger uncertainties as compared to the method that is validated here. In this manuscript, the chi-square technique that determines the most likely functional behavior is validated through numerical simulation and by application to a large body of Raman lidar measurements. In general, we show that the chi-square approach to evaluate aerosol extinction yields lower extinction uncertainty than the traditional technique. We also use the technique to study the feasibility of developing a general characterization of the extinction uncertainty that could permit the uncertainty in Raman lidar aerosol extinction measurements to be estimated accurately without the use of the chi-square technique.

Russo, Felicita↗

DOE OSTI2024

Low-Temperature Annealing of Nanoscale Defects in Polycrystalline Graphite

Polycrystalline graphite contains multi-scale defects, which are difficult to anneal thermally because of the extremely high temperatures involved in the manufacturing process. In this study, we demonstrate annealing of nuclear graphite NBG-18 at temperatures below 28 °C, exploiting the electron wind force, a non-thermal stimulus. High current density pulses were passed through the specimens with a very low-duty cycle so that the electron momentum could mobilize the defects without heating the specimen. The effectiveness of this technique is presented with a significant decrease in electrical resistivity, defect counts from X-ray computed tomography, Raman spectroscopy, and nanoindentation-based mechanical characterization. Such multi-modal evidence highlights the feasibility of nanoscale defect control at temperatures about two orders of magnitude below the graphitization temperature.

Liu, Gongyuan↗

NASA NTRS2012

Correction Technique for Raman Water Vapor Lidar Signal-Dependent Bias and Suitability for Water Wapor Trend Monitoring in the Upper Troposphere

The MOHAVE-2009 campaign brought together diverse instrumentation for measuring atmospheric water vapor. We report on the participation of the ALVICE (Atmospheric Laboratory for Validation, Interagency Collaboration and Education) mobile laboratory in the MOHAVE-2009 campaign. In appendices we also report on the performance of the corrected Vaisala RS92 radiosonde measurements during the campaign, on a new radiosonde based calibration algorithm that reduces the influence of atmospheric variability on the derived calibration constant, and on other results of the ALVICE deployment. The MOHAVE-2009 campaign permitted the Raman lidar systems participating to discover and address measurement biases in the upper troposphere and lower stratosphere. The ALVICE lidar system was found to possess a wet bias which was attributed to fluorescence of insect material that was deposited on the telescope early in the mission. Other sources of wet biases are discussed and data from other Raman lidar systems are investigated, revealing that wet biases in upper tropospheric (UT) and lower stratospheric (LS) water vapor measurements appear to be quite common in Raman lidar systems. Lower stratospheric climatology of water vapor is investigated both as a means to check for the existence of these wet biases in Raman lidar data and as a source of correction for the bias. A correction technique is derived and applied to the ALVICE lidar water vapor profiles. Good agreement is found between corrected ALVICE lidar measurments and those of RS92, frost point hygrometer and total column water. The correction is offered as a general method to both quality control Raman water vapor lidar data and to correct those data that have signal-dependent bias. The influence of the correction is shown to be small at regions in the upper troposphere where recent work indicates detection of trends in atmospheric water vapor may be most robust. The correction shown here holds promise for permitting useful upper tropospheric water vapor profiles to be consistently measured by Raman lidar within NDACC (Network for the Detection of Atmospheric Composition Change) and elsewhere, despite the prevalence of instrumental and atmospheric effects that can contaminate the very low signal to noise measurements in the UT.

MOHAVE-2009↗

DOE OSTI2024

Online Monitoring of Catalytic Processes by Fiber-Enhanced Raman Spectroscopy

An innovative solution for real-time monitoring of reactions within confined spaces, optimized for Raman spectroscopy applications, is presented. This approach involves the utilization of a hollow-core waveguide configured as a compact flow cell, serving both as a conduit for Raman excitation and scattering and seamlessly integrating into the effluent stream of a cracking catalytic reactor. The analytical technique, encompassing device and optical design, ensures robustness, compactness, and cost-effectiveness for implementation into process facilities. Notably, the modularity of the approach empowers customization for diverse gas monitoring needs, as it readily adapts to the specific requirements of various sensing scenarios. As a proof of concept, the efficacy of a spectroscopic approach is shown by monitoring two catalytic processes: CO 2 methanation (CO 2 + 4H 2 → CH 4 + 2H 2 O) and ammonia cracking (2NH 3 → N 2 + 3H 2 ). Leveraging chemometric data processing techniques, spectral signatures of the individual components involved in these reactions are effectively disentangled and the results are compared to mass spectrometry data. This robust methodology underscores the versatility and reliability of this monitoring system in complex chemical environments.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

NASA NTRS2004

A New Way to Measure Cirrus Ice Water Content by Using Ice Raman Scatter with Raman Lidar

High and cold cirrus clouds mainly contain irregular ice crystals, such as, columns, hexagonal plates, bullet rosettes, and dendrites, and have different impacts on the climate system than low-level clouds, such as stratus, stratocumulus, and cumulus. The radiative effects of cirrus clouds on the current and future climate depend strongly on cirrus cloud microphysical properties including ice water content (IWC) and ice crystal sizes, which are mostly an unknown aspect of cinus clouds. Because of the natural complexity of cirrus clouds and their high locations, it is a challenging task to get them accurately by both remote sensing and in situ sampling. This study presents a new method to remotely sense cirrus microphysical properties by using ice Raman scatter with a Raman lidar. The intensity of Raman scattering is fundamentally proportional to the number of molecules involved. Therefore, ice Raman scattering signal provides a more direct way to measure IWC than other remote sensing methods. Case studies show that this method has the potential to provide essential information of cirrus microphysical properties to study cloud physical processes in cirrus clouds.

Wang, Zhien↗

DOE OSTI2025

Reorganization of Water at Aqueous Aluminum Chloride (AlCl 3 ) Interfaces: Vibrational Sum Frequency Generation and Molecular Dynamics Simulations

AlCl 3 hydration states and complexation are not well understood both in solutions and at the air–aqueous interface despite their potential significance in natural waters and their industrial and energy-related applications. Here, we investigated Al 3+ and Cl – ion behaviors in an AlCl 3 aqueous bulk solution and at the air–aqueous interface using interface-selective vibrational sum frequency generation (SFG), Raman and infrared spectroscopies, molecular dynamics (MD) simulation, as well as molecular-informed reduced modeling. Our reduced modeling reveals relatively long-range effects for Al 3+ as compared to monovalent ions such as Na + indicating that the interfacial depth of trivalent ions can be significantly larger than that of monovalent ions at the air–water interface. MD simulations reveal interfacial stratification and multiple layering of the ions. Compression of the Al 3+ and Cl – distributions with increasing concentrations from 0.5 to 2.5 m is also observed in the subsurface regions. Significant SSP- and PPP-polarized SFG OH spectral intensity increases are observed from 0.5 to 1.5 m and 0.5 to 2.5 m, respectively, indicative of interfacial depth increases and a change in average orientation above 1.5 m. Extensive evaluation of SFG spectra, Fresnel-corrected using several approaches, shows the same trends. The nonmonotonic trend points to a changing structure in surface and subsurface water orientation and hydrogen bonding environment generally consistent with the MD simulation of stratification and water orientation changes. Furthermore, solvent-shared ion pairing is implicated with MD simulation radial distribution analysis and consistent with infrared spectral identification of the hexaaqua aluminum ion in the solution phase. Spectral evidence of a strong Al 3+ hydration shell and the acidic behavior of the Al 3+ ions is obvious in the Raman and infrared spectra of the bulk solution. In conclusion, we show that the MD dipole potential is directly related to the MD second-order susceptibility of the interface, χ SFG–MD (2) , both of which correlate up to ∼35 Å with the spectral observations of increasing and then saturating intensities, suggesting that both ion stratification and interfacial depth determine the water orientations at an air–water interface of 1-3 electrolyte solutions.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2024

Quantifying the thermal effect and methyl radical production in nanosecond repetitively pulsed glow discharges applied to a methane-air flame

In this work, we investigated non-equilibrium plasma produced by nanosecond repetitively pulsed glow discharges applied across a lean premixed methane-air flame. The flame is stationary, axisymmetric, and laminar. The discharges are applied on the symmetry axis crossing the reactant gases, flame front, and product gases, allowing phase-locked averaged measurements and comparisons with axisymmetric numerical simulations. The thermal effect and methyl radical production are quantified in the discharge in the reactant gas region. One-dimensional, two-beam, hybrid, femtosecond-picosecond, coherent anti-Stokes Raman scattering is used to acquire spatial and temporal profiles of temperature and oxygen-to-nitrogen concentration ratio. Photo-fragmentation laser-induced fluorescence is used to acquire quantitative two-dimensional profiles of methyl radicals in the discharge providing the first quantitative imaging of methyl produced ahead of a flame by plasma-induced methane dissociation. The spatial profiles of temperature and oxygen-to-nitrogen concentration ratio are in steady state, indicating that individual discharges have an insignificant heating effect. Upper and lower bounds of the produced mole fraction of methyl radicals in the plasma are obtained due to uncertainties in the collisional quenching rates of excited state methylidyne radicals in the plasma. The discharges produce a maximum of 600–1100 ppm of methyl radicals upstream of the flame front within 25 ns. This amount is similar to the predicted methyl mole fraction for the flame without plasma and thus represents a significant chemical perturbation to the reactants upstream of the flame front. The produced methyl follows an exponential decay in the first microsecond after the discharge with a decay constant of 8 µs close to the flame, and 0.8 µs further from the flame. The decay then deviates from the exponential curve and the methyl persists for tens of microseconds. The results suggest that for the tested configuration, the thermal effect of individual discharges through fast gas heating is negligible, while active chemical species are produced in large quantities in the reactant gases, upstream of the flame front.

hybrid fs-ps CARS↗

DOE OSTI2025

Dehydrogenation vs Apparent Hydrogenation: Unraveling the Mechanisms of He and O 2 Plasma Etching on Colloidal Nanocrystal Films

Removing organic ligands from colloidal nanoparticles is critical for fabricating solid-state devices, yet accurately quantifying this removal remains a significant analytical challenge. Here, we establish a robust and accessible method for this quantification by calibrating Raman spectroscopy against precise ion beam analysis (IBA) for nanoparticle assemblies (CNAs) processed by helium (He) and oxygen (O 2 ) plasmas. We demonstrate that the calibration curves are remarkably independent of plasma power and pressure, depending critically only on the choice of feed gas. He plasma induces rapid dehydrogenation and cross-linking, evidenced by a much faster decrease in the C–H Raman signal relative to the actual carbon loss. Conversely, O 2 plasma leads to a surprising “apparent hydrogenation”, where the carbon backbone is removed significantly faster than the C–H signal diminishes. This counterintuitive effect is explained by a serial mechanism of oxidative fragmentation; β-scission cleaves the alkyl chains, and subsequent stabilization steps enrich the remaining film with hydrogen-rich methyl-terminated fragments, while carbon is efficiently removed as volatile CO. This work provides calibrated functions that enable the rapid determination of absolute carbon content in processed CNAs using simple Raman spectroscopy with uncertainties of ∼8% for O 2 and ∼12% for He plasma, offering a vital tool for both process diagnostics and fundamental studies of plasma–matter interactions in colloidal nanocrystal films.

Animal feed↗

NASA NTRS1993

Monte Carlo and experimental studies of nozzle flow in a low-power hydrogen arcjet

The flow in the nozzle of a small hydrogen arcjet intended for low-thrust propulsion is studied without arc ignition using numerical and experimental techniques. The flow conditions in the thruster indicate that low-density nonequilibrium effects will significantly influence the flow. Therefore, the numerical analysis is undertaken using a Monte Carlo approach. The experimental studies employ laser Raman scattering. Comparisons of the measured and computed results are made for total number density, rotational temperature, and for the number density of the first rotational level. The numerical results are found to be quite sensitive to the rotational relaxation rate, and a strong degree of thermal nonequilibrium is observed at the exit plane of the nozzle. Successful comparisons between experiment and analysis permit estimation of the rotational relaxation rate for hydrogen.

Boyd, Iain D.↗