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NASA NTRSDate not supplied

Examination of Lunar Regolith Simulants By SEM-EDS and Imaging Raman Spectroscopy

The Artemis series lunar missions will include sample returns from the lunar south pole. Lunar regolith simulants (RS) generated in the lab provide opportunities to compare two surface science techniques: scanning electron microscopy (SEM-EDS) and Raman induced surface spectroscopy. The results will also be applicable for supporting future commercial lunar payload services (CLPS) and Artemis surface. Surface characterization contributes to continued development of lunar regolith studies and adds to various regolith databases. In characterizing various lunar regolith simulants, part of the aim should be to standardize techniques and utilize anticipated methods available for astromaterials studied during, or returned from, upcoming missions, particularly samples collected from the Moon’s south pole and permanently shadowed regions (PSRs).. An initial survey of available simulants has been started with Raman scanning process for particle counting the results of which will enrich the NASA-JSC Simulant Development Lab (SDL) simulant properties database and the Colorado School of Mines Planetary Simulant Data Base. An SEM-EDS dataset of raw regolith simulant materials are collected.

Raman Microscopy↗
NASA NTRS1990

UV Raman spectroscopy of H2-air flames excited with a narrowband KrF laser

Raman spectra of H2 and H2O in flames excited by a narrowband KrF excimer laser are reported. Observations are made over a porous-plug, flat-flame burner reacting H2 in air, fuel-rich with nitrogen dilution to control the temperature, and with an H2 diffusion flame. Measurements made from UV Raman spectra show good agreement with measurements made by other means, both for gas temperature and relative major species concentrations. Laser-induced fluorescence interferences arising from OH and O2 are observed in emission near the Raman spectra. These interferences do not preclude Raman measurements, however.

Shirley, John A.↗
NASA NTRS1982

High-resolution continuous-wave coherent anti-Stokes Raman spectroscopy in a supersonic jet

High-resolution CW coherent anti-Stokes Raman spectra of the nu1 Q branch of methane in an underexpanded supersonic jet were obtained at temperatures as low as 31.5 K and pressures as low as 2 torr. The experimental spectra were well fitted by the calculated theoretical spectra, including transit-time broadening. A temperature of 31.5 K produced the best fit to the data, and the transit-time broadening was comparable to the residual Doppler broadening of about 100 MHz. The supersonic jet provides a convenient method of obtaining molecular cooling at relatively high density, and the ease of construction and the wide range of temperatures and densities available make it a useful tool for high resolution molecular spectroscopy.

Gustafson, E. K.↗
NASA NTRS2002

Hydrocarbon-Fueled Rocket Plume Measurement Using Polarized UV Raman Spectroscopy

The influence of pressure upon the signal strength and polarization properties of UV Raman signals has been investigated experimentally up to pressures of 165 psia (11 atm). No significant influence of pressure upon the Raman scattering cross section or depolarization ratio of the N2 Raman signal was found. The Raman scattering signal varied linearly with pressure for the 300 K N2 samples examined, thus showing no enhancement of cross section with increasing pressure. However at the highest pressures associated with rocket engine combustion, there could be an increase in the Raman scattering cross section, based upon others' previous work at higher pressures than those examined in this work. The influence of pressure upon thick fused silica windows, used in the NASA Modular Combustion Test Article, was also investigated. No change in the transmission characteristics of the windows occurred as the pressure difference across the windows increased from 0 psig up to 150 psig. A calibration was performed on the UV Raman system at Vanderbilt University, which is similar to the one at the NASA-Marshall Test Stand 115. The results of this calibration are described in the form of temperature-dependent functions, f(T)'s, that account for the increase in Raman scattering cross section with an increase in temperature and also account for the reduction in collected Raman signal if wavelength integration does not occur across the entire wavelength range of the Raman signal. These functions generally vary only by approximately 10% across their respective temperature ranges, except for the case Of CO2, where there is a factor of three difference in its f(T) from 300 K to 2500 K. However this trend for CO2 is consistent with the experimental work of others, and is expected based on the low characteristic vibrational temperature Of CO2. A time-averaged temperature measurement technique has been developed, using the same equipment as for the work mentioned above, that is based upon high-spectral resolution UV Raman scattering. This technique can provide temperature measurements for flows where pressure cannot be measured.

Wehrmeyer, Joseph A.↗
NASA NTRS1995

Raman Spectroscopy as a Method for Mineral Identification on Lunar Robotic Exploration Missions

The sharp, nonoverlapping Raman bands for plagioclase, pyroxene, and olivine would be advantageous for on-surface, active mineralogical analysis of lunar materials. A robust, light-weight, low-power, rover-based Raman spectrometer with a laser exciting source, entirely transmission-mode holographic optics, and a charge-coupled device (CCD) detector could fit within a less than 20 cm cube. A sensor head on the end of an optical fiber bundle that carried the laser beam and returned the scattered radiation could be placed against surfaces at any desired angle by a deployment mechanism; otherwise, the instrument would need no moving parts. A modem micro-Raman spectrometer with its beam broadened (to expand the spot to 50-micrometer diameter) and set for low resolution (7/cm in the 100-1400/cm region relative to 514.5-nm excitation), was used to simulate the spectra anticipated from a rover instrument. We present spectra for lunar mineral grains, less than 1 mm soil fines, breccia fragments, and glasses. From frequencies of olivine peaks, we derived sufficiently precise forsterite contents to correlate the analyzed grains to known rock types and we obtained appropriate forsterite contents from weak signals above background in soil fines and breccias. Peak positions of pyroxenes were sufficiently well determined to distinguish among orthorhombic, monoclinic, and triclinic (pyroxenoid) structures; additional information can be obtained from pyroxene spectra, but requires further laboratory calibration. Plagioclase provided sharp peaks in soil fines and most breccias even when the glass content was high.

Wang, Alian↗
NASA NTRS1979

Coherent anti-Stokes Raman spectroscopy - Spectra of water vapor in flames

The results of experimental measurements of the coherent anti-Stokes Raman spectra of water vapor in flames are reported. A pulsed, frequency-doubled neodymium laser was used to supply the pump beam and to pump a dye laser to provide a broadband Stokes beam at 6600 A. Spectra were obtained in the postflame region of a premixed methane-air flame in the Raman frequency shift region of the symmetric stretch mode (3651.7 kaysers) at an approximate temperature of 1675 K. A theoretical calculation of the coherent anti-Stokes Raman spectrum of water vapor at this temperature was made, taking into account only isotropic Q-branch transitions, and using the energy level data of Floud et al. (1976). The theoretical prediction is shown essentially to reproduce all qualitative features of the experimental spectrum, and to exhibit a strong temperature dependence.

Hall, R. J.↗
NASA NTRS1984

Intensified silicon photodiode array detector linearity Application to coherent anti-Stokes Raman spectroscopy

The linearity of an intensified silicon photodiode array multichannel detector is studied with coherent anti-Stokes Raman and other similar signals. Studies with diffuse and focused (spherically and cylindrically) signals resolved apparent saturation problems which limit the dynamic range of the detector. In addition, it has been shown that there is no short-range wavelength (473-532-nm) dependence on this saturation. Theoretical explanations for these phenomena are also included.

Antcliff, R. R.↗
NASA NTRS2003

Metallized Capillaries as Probes for Raman Spectroscopy

A class of miniature probes has been proposed to supplant the fiber-optic probes used heretofore in some Raman and fluorescence spectroscopic systems. A probe according to the proposal would include a capillary tube coated with metal on its inside to make it reflective. A microlens would be hermetically sealed onto one end of the tube. A spectroscopic probe head would contain a single such probe, which would both deliver laser light to a sample and collect Raman or fluorescent light emitted by the sample.

Pelletier, Michael↗
NASA NTRS2008

Low-Resolution Raman-Spectroscopy Combustion Thermometry

A method of optical thermometry, now undergoing development, involves low-resolution measurement of the spectrum of spontaneous Raman scattering (SRS) from N2 and O2 molecules. The method is especially suitable for measuring temperatures in high pressure combustion environments that contain N2, O2, or N2/O2 mixtures (including air). Methods based on SRS (in which scattered light is shifted in wavelength by amounts that depend on vibrational and rotational energy levels of laser-illuminated molecules) have been popular means of probing flames because they are almost the only methods that provide spatially and temporally resolved concentrations and temperatures of multiple molecular species in turbulent combustion. The present SRS-based method differs from prior SRS-based methods that have various drawbacks, a description of which would exceed the scope of this article. Two main differences between this and prior SRS-based methods are that it involves analysis in the frequency (equivalently, wavelength) domain, in contradistinction to analysis in the intensity domain in prior methods; and it involves low-resolution measurement of what amounts to predominantly the rotational Raman spectra of N2 and O2, in contradistinction to higher-resolution measurement of the vibrational Raman spectrum of N2 only in prior methods.

Nguyen, Quang-Viet↗
NASA NTRS2017

Method of Stamping Surface-Enhance Raman Spectroscopy for Label-Free, Multiplexed, Molecular Sensing and Imaging

The present disclosure relates the use of a stamping surface enhanced Raman scattering (S-SERS) technique with nanoporous gold disk (NPGD) plasmonic substrates to produce a label-free, multiplexed molecular sensing and imaging technique. A NPGD SERS substrate is stamped onto a surface containing one or more target molecules, followed by SERS measurement of the target molecules located between the surface and SERS substrate. The target molecules may be deposited on the surface, which may be a carrier substrate such as polydimethylsiloxane (PDMS).

Shih, Wei-Chuan↗
NASA NTRS2003

Material for surface-enhanced Raman spectroscopy, and SER sensors and method for preparing same

Metal-doped sol-gel materials, suitable for use as sensors for surface-enhanced Raman spectroscopic analysis for trace chemical detection, are produced by effecting gelation and solvent removal of a doped sol-gel under mild temperature conditions. At least in certain instances reaction and drying will desirably be effected in an oxygen-starved environment. The metal of the sol-gel material functions, when irradiated, to produce a plasmon field for interaction with molecules of an analyte in contact therewith, increasing by orders of magnitude Raman photons that are generate by excitation radiation, and the method allows matching of the metal and metal particle size to a wavelength of light (or incident radiation, e.g., laser radiation) to generate surface plasmons. The porosity of the sol-gel material dramatically increases the surface area, and thereby the amount of metal exposed for analyte interaction. The sensors provided may be in the form of glass vials, fiber optics, multi-well micro-sample plates, etc., having surface coatings of the doped sol-gel material, to provide sampling systems for use in a Raman instrument.

Farquharson, Stuart↗
NASA NTRS1999

Raman Spectroscopy for Instantaneous Multipoint, Multispecies Gas Concentration and Temperature Measurements in Rocket Engine Propellant Injector Flows

Propellent injector development at MSFC includes experimental analysis using optical techniques, such as Raman, fluorescence, or Mie scattering. For the application of spontaneous Raman scattering to hydrocarbon-fueled flows a technique needs to be developed to remove the interfering polycyclic aromatic hydrocarbon fluorescence from the relatively weak Raman signals. A current application of such a technique is to the analysis of the mixing and combustion performance of multijet, impinging-jet candidate fuel injectors for the baseline Mars ascent engine, which will bum methane and liquid oxygen produced in-situ on Mars to reduce the propellent mass transported to Mars for future manned Mars missions. The present technique takes advantage of the strongly polarized nature of Raman scattering. It is shown to be discernable from unpolarized fluorescence interference by subtracting one polarized image from another. Both of these polarized images are obtained from a single laser pulse by using a polarization-separating calcite rhomb mounted in the imaging spectrograph. A demonstration in a propane-air flame is presented.

Wehrmeyer, Joseph A.↗
NASA NTRS2001

Raman Spectroscopy for Instantaneous Multipoint, Multispecies Gas Concentration and Temperature Measurements in Rocket Engine Propellant Injector Flows

Propellant injector development at MSFC includes experimental analysis using optical techniques, such as Raman, fluorescence, or Mie scattering. For the application of spontaneous Raman scattering to hydrocarbon-fueled flows a technique needs to be developed to remove the interfering polycyclic aromatic hydrocarbon fluorescence from the relatively weak Raman signals. A current application of such a technique is to the analysis of the mixing and combustion performance of multijet, impinging-jet candidate fuel injectors for the baseline Mars ascent engine, which will burn methane and liquid oxygen produced in-situ on Mars to reduce the propellant mass transported to Mars for future manned Mars missions. The present technique takes advantage of the strongly polarized nature of Raman scattering. It is shown to be discernable from unpolarized fluorescence interference by subtracting one polarized image from another. Both of these polarized images are obtained from a single laser pulse by using a polarization-separating calcite rhomb mounted in the imaging spectrograph. A demonstration in a propane-air flame is presented.

Wehrmeyer, Joseph A.↗
NASA NTRS1980

Coherent Anti-stokes Raman Spectroscopy (CARS) of gun propellant flames

Temperature measurements were made in a slightly fuel rich, premixed propane/air reference flame and nitrate ester propellant flames burning in air at atmospheric pressure using coherent anti-stokes raman scattering (CARS). Both single and multiple pulse VARS spectra of nitrogen in the reference flame were in good agreement with calculated and reported values. Single pulse CARS nitrogen spectra obtained in the propellant flames were analyzed to give temperatures consistent with values calculated using the NASA-Lewis thermochemical calculation. Comparison of a 0.1 second separated sequence of single pulse CARS spectra indicate turbulent air mixing in these propellant flames. The CARS spectral results demonstrate that temporal and spatially resolved temperature measurements could be determined in transient, turbulent flames.

Mcilwain, M. E.↗
NASA NTRS2003

In-SITU Raman Spectroscopy of Single Microparticle Li-Intercalation Electrodes

Modifications in the vibrational properties of a single microparticle of LiMn2O4 induced by extraction and subsequent injection of Li(+) into the lattice have been monitored in situ via simultaneous acquisition of Raman scattering spectra and cyclic voltammetry data in 1M LiC1O4 solutions in ethylene carbonate (EC):diethyl carbonate (DEC) mixtures (1:1 by volume). Statistical analyses of the spectra in the range 15 < SOD < 45%, where SOD represents the state of discharge (in percent) of the nominally fully charged material, i.e. lambda-MnO2, were found to be consistent with the coexistence of two distinct phases of lithiated metal oxide in agreement with information derived from in situ X-ray diffraction (XRD) measurements involving more conventional battery-type electrodes.

Dokko, Kaoru↗
NASA NTRS1985

Micro-Raman spectroscopy: The analysis of micrometer and submicrometer atmospheric aerosols

A nondestructive method of molecular analysis which is required to fully utilize the information contained within a collected particle is discussed. Upper atmosphere reaction mechanisms are assessed when the chemical compounds, the use of micro-Raman spectrometric techniques to perform micron and submicron particle analysis was evaluated. The results are favorable and it is concluded that micron and submicron particles can be analyzed by the micron-Raman approach. Completely automatic analysis should be possible to 0.3 micro m. No problems are anticipated with photo or thermal decomposition. Sample and impurity fluorescence are the key source of background as they cannot be completely eliminated.

Klainer, S. M.↗
NASA NTRS2003

A Study of Olivine Alteration to Iddingsite Using Raman Spectroscopy

A crucial task of Mars surface science is to determine past environmental conditions, especially aqueous environments and their nature. Identification of mineral alteration by water is one way to do this. Recent work interprets TES spectra as indicating altered basalt on Mars. Olivine, a primary basaltic mineral, is easily altered by aqueous solutions. Alteration assemblages of olivine may be specific to deuteric, hydrothermal, surface water, or metamorphic environments. Raman spectra are produced by molecular vibrations and provide direct means for studying and identifying alteration products. Here, we present a combined study of changes in the chemical composition and Raman spectra of an olivine as it alters to iddingsite. Iddingsite is found in some SNC meteorites and is presumably present on Mars. The term 'iddingsite' has been used as a catch-all term to describe reddish alteration products of olivine, although some authors ascribe a narrower definition: an angstrom-scale intergrowth of goethite and smectite (presumably saponite) formed in an oxidizing and fluid-rich environment. Alteration conserves Fe (albeit oxidized) but requires addition of Al and H2O and removal of Mg and Si. The smectite that forms may be removed by continued alteration. Dehydration of the goethite forms hematite. Our purpose is to study the mineral assemblage, determine the structural and chemical variability of the components with respect to the degree of alteration, and to find spectral indicators of alteration that will be useful during in-situ analyses on Mars.

Kuebler, K. E.↗