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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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Microstructural Constraints on the Formation of Diamond in Ureilites, the Case from the Kenna Meteorite

The origin of diamonds in ureilitic meteorites, a major family of ultramafic achondrites, has long been debated, with various formation mechanisms inferred, including: 1) shock conversion of preexisting graphite due to a hypervelocity impact on the ureilite parent body; 2) vapor deposition during condensation of the solar nebula; or 3) static transformation in the mantle of a large planetesimal (>1000 km in diameter). The Kenna ureilite is a 10.9 kg stone that was found in Kansas in 1972 and is dominantly composed of olivine and pigeonite (68% and 22% modal abundance, respectively), together with minor metal and carbon-rich regions. Within the carbon-rich domains researchers have identified microdiamonds up to ~10 µm in size. Due to the proximity of the extremely hard microdiamonds with soft graphite and moderately hard silicates, achieving an appropriately flat surface for electron backscatter diffraction (EBSD) analysis has proved challenging. We have, therefore, employed a Hitachi ArBlade 5000 broad beam Ar ion milling system to prepare a sample with an adequate surface uniformity. The ion milling dramatically improved indexing of the EBSD patterns and facilitated high-resolution microstructural analysis of the carbon-rich domains. The carbon-bearing regions occur as tabular domains between polygonal olivine and pigeonite, and are composed of aggregates of micrometer-scale diamond with intermediate graphite, oxides and metal grains. Within the microdiamonds, {111} twins are abundant, many of which form ragged lamellae consistent with mechanical twinning. The microdiamond assemblages appear to pseudomorph tabular graphite habits, which together with the abundant deformation twins, supports a shock transformation mechanism for microdiamond formation within the Kenna meteorite. To compliment the EBSD microstructural analyses, coordinated laser Raman, focused ion beam/transmission electron microscopy imaging and diffraction data, and NanoSIMS N and C tomographic isotopic imaging will be collected. These data will provide further constraints on the formation of diamonds within ureilites.

Timmons M Erickson↗
DOE OSTI2024

Characterization of SimulCam, a standoff Raman system for scientific support of SuperCam operations on Mars

During the development activities of SuperCam Calibration Target, target intended for one of the two first Raman instruments to be deployed on another planetary body, our group developed a laboratory instrument that could simulate to some extent the Raman capabilities of one of such instruments and could provide data with similar quality. The use of this kind of laboratory instruments has demonstrated its utility in the evaluation of potential calibration targets or anticipating the science outcome that an instrument could provide. The present work describes our laboratory setup to support SuperCam, evaluating similarities between both instruments, despite of differences in the hardware. Evaluation of data gathered by SuperCam on Mars and the availability of one replica of SuperCam’s Calibration Target allowed the comparison on the same set of targets, demonstrating how similar Signal-to-Noise Ratio (SNR) could be achieved from both instruments. The higher energy per pulse on SimulCam is compensated by a greater analytical footprint and the use of smaller collection optics. The results show how spectra obtained at representative distances of SuperCam are comparable. Operational principles are also comparable in terms of time resolution, and close in terms of spectral resolution. This similarity has allowed different science support works using SimulCam data, as well as the support to Mars detections using our setup. We provide examples of this support that will be shared with the community in different papers, as well as examples of possible operations activities that could benefit from experiments performed with SimulCam. We show how this setup can complement the two laboratory replicas in Los Alamos and Toulouse in providing support data to different experiments.

47 OTHER INSTRUMENTATION↗
DOE OSTI2020

TORONE: Total Characterisation by Remote Observation of Nuclear Environments - 20591

This paper describes the autonomous robotic systems developed in the TORONE project (Total Characterisation by Remote Observation of Nuclear Environments) for combined characterisation by remote techniques in nuclear environments. There are four main components to the system. Firstly, robot operation which uses a Robot Operating System (ROS) allowing ease of communication between hardware and software alongside robot vision systems such as Lidar and/or photogrammetry. Secondly, radiation detection instrumentation for gamma and neutron sources which is also collimated for spatial resolution. Thirdly, photonic characterisation instrumentation for remote material identification by means of Raman spectroscopy and Laser induced breakdown spectroscopy (LIBS). Finally, a data management system is described which contains the TORONE characterisation data with the ability to overlay material characterisation information onto 3D maps of the nuclear environment. Preliminary results are described alongside discussion of some of the synergies of the combined approach. There are many applications of such an autonomous system in nuclear decommissioning, waste management and asset management. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
NASA NTRS1973

Remote Measurement of Atmospheric Temperatures By Raman Lidar

The Raman shifted return of a lidar, or optical radar, system has been utilized to make atmospheric temperature measurements. These measurements were made along a horizontal path at temperatures between -20 C and +30 C and at ranges of about 100 meters. The temperature data were acquired by recording the intensity ratio of two portions of the Raman spectrum which were simultaneously sampled from a preset range. The lidar unit employed in this testing consisted of a 4 joule-10ppm laser operating at 694.3 nm, a 10-inch Schmidt-Cassegrain telescope, and a system of time-gated detection and signal processing electronics. The detection system processed three return signal wavelength intervals - two intervals along the rotational Raman scattered spectrum and one interval centered at the Rayleigh-Mie scattered wavelength. The wavelength intervals were resolved by using a pellicle beam splitter and three optical interference filters. Raman return samples were taken from one discrete range segment during each test shot and the signal intensities were displayed in digital format. The Rayleigh-Mie techniques. The test site utilized to evaluate this measurement technique encompassed a total path length of 200 meters. Major components of the test site included a trailer-van housing the lidar unit, a controlled environment test zone, and a beam terminator. The control zone which was located about 100 meters from the trailer was 12 meters in length, 2.4 meters in diameter, and was equipped with hinged doors at each end. The temperature of the air inside the zone could be either raised or lowered with respect to ambient air through the use of infrared heaters or a liquid-nitrogen cooling system. Conditions inside the zone were continuously monitored with a thermocouple rake assembly. The test path length was terminated by a 1.2 meter square array of energy absorbing cones and a flat black screen. Tests were initially conducted at strictly ambient conditions utilizing the normal outside air temperatures as a test parameter. These tests provided a calibration of the Raman intensity ratio as a function of' temperature for the particular optical-filter arrangement used in this system while also providing a test of' the theoretical prediction formulated in the design of the system. Later tests utilized zone temperatures above and below ambient to provide temperature gradient data. These tests indicate that ten shots, or one minute of' data acquisition, from a 100 meter range can provide absolute temperature measurements with an accuracy of + 30 C and a range resolution of about 5 meters. Because this measurement accuracy compares well with that predicted for this particular unit, it is suggested that a field-application system could be built with signif'icant improvements in both absolute accuracy and range.

Salzman, Jack A.↗
DOE OSTI2023

Development of a continuous synthesis process for carbamazepine using validated in-line Raman spectroscopy and kinetic modelling for disturbance simulation

Mitigation of failure modes in the continuous synthesis (CS) of a drug substance (DS) has the potential to widen the adoption of continuous manufacturing (CM) technologies by the pharmaceutical industry. Here, this work demonstrates the development of a robust continuous process for the synthesis of carbamazepine (CBZ), an essential medicine as per the World Health Organization (WHO), facilitated by kinetic modelling and monitored by in-line Raman spectroscopy. Accurate kinetic modelling and the use of validated process analytical technology (PAT) models for quantitative measurement were found to play an important role in developing CS of drug substances. Kinetic data for the formation of CBZ from iminostilbene (ISB) were collected by batch reaction sampling and high-performance liquid chromatography (HPLC) analysis. A non-linear solver and iterative method was applied to determine two sets of Arrhenius parameters simultaneously for the reaction system by minimizing the standard error of the model fit. The start-up and dynamic equilibrium stages for the CS of CBZ using a continuous stirred tank reactor (CSTR) were modelled based on the batch kinetic data and employed to optimize conversion and simulate process disturbances. An in-line Raman spectroscopy method was successfully developed, validated, and integrated to determine the concentrations of CBZ and ISB within the operating range for the CS. The CS kinetic model was evaluated experimentally from startup to dynamic equilibrium over 10 residence times with monitoring by HPLC and in-line Raman spectroscopy. The developed kinetic model in tandem with in-line Raman spectroscopy successfully predicted disturbances due to changes in process variables and can serve as a useful tool in the future design of advanced process control strategies for the continuous synthesis of CBZ.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
NASA NTRS2008

Demonstration of Aerosol Property Profiling by Multi-wavelength Lidar Under Varying Relative Humidity Conditions

The feasibility of using a multi-wavelength Mie-Raman lidar based on a tripled Nd:YAG laser for profiling aerosol physical parameters in the planetary boundary layer (PBL) under varying conditions of relative humidity (RH) is studied. The lidar quantifies three aerosol backscattering and two extinction coefficients and from these optical data the particle parameters such as concentration, size and complex refractive index are retrieved through inversion with regularization. The column-integrated, lidar-derived parameters are compared with results from the AERONET sun photometer. The lidar and sun photometer agree well in the characterization of the fine mode parameters, however the lidar shows less sensitivity to coarse mode. The lidar results reveal a strong dependence of particle properties on RH. The height regions with enhanced RH are characterized by an increase of backscattering and extinction coefficient and a decrease in the Angstrom exponent coinciding with an increase in the particle size. We present data selection techniques useful for selecting cases that can support the calculation of hygroscopic growth parameters using lidar. Hygroscopic growth factors calculated using these techniques agree with expectations despite the lack of co-located radiosonde data. Despite this limitation, the results demonstrate the potential of multi-wavelength Raman lidar technique for study of aerosol humidification process.

Whiteman, D.N.↗
DOE OSTI2021

Tunable structural, morphological and optical properties of undoped, Mn, Ni and Ag-doped CuInS 2 thin films prepared by AACVD

The preparation of high-quality copper indium sulphide, CuInS 2 photo-absorber material with tunable properties for efficient, low-cost, thin film solar cells using scalable methods remains a challenge. In order to address this, high quality off-stoichiometric undoped and Mn, Ni and Ag-doped CuInS 2 (CIS) thin films have been deposited onto glass substrates by aerosol-assisted chemical vapour deposition (AACVD) using metal diethyldithiocarbamate precursors at temperatures of 350, 400 and 450 °C. Data from powder X-ray diffraction (p-XRD), Raman spectroscopy and scanning electron microscopy-energy dispersive X-ray spectroscopy (SEM-EDS) suggest a correlation of morphology and composition of tetragonal phase (chalcopyrite and copper-gold-type) sulphur-deficient microcrystalline CIS thin films. For undoped thin films, near-infrared optical absorption and emission with tunable band gap between 1.32 and 1.42 eV are likely associated with donor-acceptor pairs involving deep or shallow electronic states such as sulphur vacancies (V S •• ), indium-copper anti-sites (In Cu •• ) and indium interstitials (In i ••• ) as donors and copper vacancies (V Cu ') as acceptors. Whilst Mn-doped thin films exhibit minimal tunable properties, Ni and Ag-doped films exhibit tunable morphology, composition and near-infrared absorption for small dopant content. Here, though further studies are required to explore the defect chemistry, these results show the utility of AACVD in tuning structural, morphological and optical properties of undoped, Mn, Ni and Ag-doped CIS thin films.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Lattice Dynamics and Structural Phase Transitions in Eu 2 O 3

Using the density functional theory, we study the structural and lattice dynamical properties of europium sesquioxide (Eu 2 O 3 ) in the cubic, trigonal, and monoclinic phases. The obtained lattice parameters and energies of the Raman modes show a good agreement with the available experimental data. The Eu-partial phonon density of states calculated for the cubic structure is compared with the nuclear inelastic scattering data obtained from a 20 nm thick Eu 2 O 3 film deposited on a YSZ substrate. A small shift of the experimental spectrum to higher energies results from a compressive strain induced by the substrate. On the basis of lattice and phonon properties, we analyze the mechanisms of structural transitions between different phases of Eu 2 O 3 .

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

Evaluation of Changes to the MTR Fuel Dissolution Flowsheet to Increase the Number of L-Bundles Charged to a Dissolver

Material Test Reactor (MTR) fuels are dissolved in the H-Canyon facility using a Hg-catalyzed, HNO₃ dissolution flowsheet. The flowsheet is based on experimental work in which laboratory-scale experiments were used to provide bounding values for both offgas and H₂ generation rates. The generation of H₂ gas, primarily from the dissolution of Al, is controlled by limiting the surface area exposed to the solution. The number of L-Bundles charged and their submergence level defines the exposed surface area which is directly proportional to the H₂ generation rate. For the MTR fuel dissolution flowsheet, the maximum number of L-Bundles which can be charged to a dissolver was specified as a function of the Al concentration in the solution and the submergence level of the bundle. The MTR fuels are currently dissolved in the 6.1D dissolver. To reach the desired terminal Al concentration, a total of 12 L-Bundles of fuel are dissolved per batch. Depending on the submergence level being used in the dissolver, the 12 bundles are dissolved in three charges of four bundles per charge or in a sequence of three, four, and five bundles. However, if six L-Bundles could be dissolved in the initial charge, a dissolver batch could be completed in two dissolutions instead of three. To assess the feasibility of dissolving six bundles in the first charge, the Savannah River National Laboratory evaluated changes to the MTR flowsheet which increase the number of bundles which can be charged to a dissolver. Since the development of the existing MTR fuel dissolution flowsheet, improved offgas measurement methods have been developed to more accurately calculate the offgas composition and generation rate during laboratory-scale dissolutions. In the first part of this study, improvements in the calibration model for the Raman spectrometer (used for offgas characterization) and a more effective data smoothing routine were applied to existing data. The uncertainty in the offgas composition data used to define the MTR fuel dissolution flowsheet were subsequently re-evaluated which resulted in an approximate 50% reduction in the uncertainty of the H₂ gas concentration measurements. The reduced uncertainty was used in new calculations to define the maximum number of L-Bundles which can be charged to either the 6.1D or 6.4D dissolver as a function of the Al concentration. With the reduced uncertainty in the H₂ concentration measurements, a flowsheet was defined which supported initially charging 6 bundles to a dissolver. This flowsheet is based on the use of 0.002 M Hg, an L-Bundle immersion depth of 54 in., an air sparge/purge flowrate of 40 scfm, an iodine reactor operating temperature of 200 °C, and not exceeding 60% of the H₂ LFL in the dissolver offgas. In the second phase of this study, calculations were performed to assess the impact of changing various operating parameters to increase the number of L-Bundles charged to an H-Canyon dissolver. Applying the improved offgas measurement techniques including the reduced uncertainty in the H₂ concentration measurements to the existing data, the number of bundles of MTR fuel which can be charged to either the 6.1D or 6.4D dissolver were calculated based on varying the bundle immersion depth (44-60 in.), air sparge/purge flowrate (40-60 scfm), iodine reactor operating temperature (150-200 °C), and the percentage of the H₂ LFL which must not be exceeded (60-76%). Qualitatively, the percentage of the LFL had the largest influence on the maximum number of bundles which can be charged to a dissolver followed by the air sparge/purge flowrate, L-Bundle immersion depth, and the iodine reactor operating temperature. During the evaluation of each variable, the other variables were held at the baseline flowsheet conditions.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
NASA NTRS1998

Detailed Experimental Data for CFD Code Validation

Recent interest in low cost, reliable access to space has generated increased interest in advanced technology approaches to space transportation systems. A key to the success of such programs lies in the development of advanced propulsion systems capable of achieving the performance and operations goals required for the next generation of space vehicles. One extremely promising approach involves the combination of rocket and air-breathing engines into a rocket-based combined-cycle engine (RBCC). A key element of that engine is the rocket ejector that is utilized in the zero to Mach two operating regime. Studies of RBCC engine concepts are not new and studies dating back thirty years are well documented in the literature. However, studies focused on the rocket ejector mode of the RBCC cycle are lacking. The present investigation utilizes an integrated experimental and computation fluid dynamics (CFD) approach to examine critical rocket ejector performance issues. In particular, the development of a predictive methodology capable of performance prediction is a key objective in order to analyze thermal choking and its control, primary/secondary pressure matching considerations, and effects of nozzle expansion ratio. To achieve this objective, the present study emphasizes obtaining new data using advanced optical diagnostics such as Schlieren photography and Raman spectroscopy, and CFD techniques to investigate mixing in the rocket ejector mode. A new research facility for the study of the rocket ejector mode has been developed. In the last milestone report, the operational capabilities of this research facility were described. In this milestone report, the experimentally obtained measurements for CFD code validation are presented and discussed.

Santoro, Robert J.↗
NASA NTRS2008

Progress on the Use of Combined Analog and Photon Counting Detection for Raman Lidar

The Atmospheric Radiation Measurement (ARM) program Raman Lidar (CARL) was upgraded in 2004 with a new data system that provides simultaneous measurements of both the photomultiplier analog output voltage and photon counts. The so-called merge value added procedure (VAP) was developed to combine the analog and count-rate signals into a single signal with improved dynamic range. Earlier versions of this VAP tended to cause unacceptably large biases in the water vapor mixing ratio during the daytime as a result of improper matching between the analog and count-rate signals in the presence of elevated solar background levels. We recently identified several problems and tested a modified version of the merge VAP by comparing profiles of water vapor mixing ratio derived from CARL with simultaneous sonde data over a six month period. We show that the modified merge VAP significantly reduces the daytime bias, and results in mean differences that are within approximately 1% for both nighttime and daytime measurements.

Newsom, Rob↗
DOE OSTI2026

Evaluating Limits of Machine Learning-Assisted Raman Spectroscopy in Classification of Biological Samples

Machine learning (ML)-assisted Raman spectroscopy has become a powerful analytical tool for the classification and identification of analytes; however, technical challenges impacting its detection accuracy have not been thoroughly investigated. This study explores experimental factors affecting classification performance. Among the evaluated ML models, ML algorithms show minimal impact on classification accuracy. Instead, experimental factors, including spectral similarity between tested samples and data quality, dominate detection performance. Increases in spectral noise and spectral similarity significantly reduce classification accuracy. In well-controlled samples with low experimental noise, ML-assisted Raman spectroscopy can discriminate lipid mixtures with a composition difference of 1.85 mol %. To assess the effect of biological heterogeneity, we analyzed single-cell Raman spectra from Saccharomyces cerevisiae strains carrying single, double, or triple gene mutations. Intrinsic cell-to-cell variability introduced substantial spectral differences, severely reducing the accuracy of multiclass classification of these genetically similar strains at the single-cell level. Averaging Raman spectra across multiple cells improved classification accuracy by reducing this spectral variability. We also assess the effectiveness of transfer learning across different Raman spectrometers, specifically by applying an ML model trained on one instrument to another Raman spectrometer. Transfer learning can be improved with proper instrument calibration, highlighting the importance of instrument standardization. Overall, our results demonstrate that data quality and spectral similarity are the primary bottlenecks in ML-assisted Raman spectroscopy. Careful attention to sample preparation, data acquisition, measurement conditions, and instrument calibration is critical to achieving robust and reliable classification performance.

Fungi↗
NASA NTRS1973

Remote measurement of atmospheric temperatures by Raman lidar

The Raman shifted return of a lidar system was utilized to make atmospheric temperature measurements. The measurements were made along a horizontal path at temperatures between -20 and +30 C and at ranges of about 100 meters. The temperature data were acquired by recording the intensity ratio of two portions of the rotational Raman spectrum which were simultaneously sampled from a preset range. Measurements were made to an accuracy of + or - 3 C with 1 minute temporal resolution.

Salzman, J. A.↗
DOE OSTI2026

A comparative study of multimodal data fusion strategies for planetary spectroscopy

Integrating heterogeneous data sources can improve scientific inference when different modalities capture complementary information, but doing so is challenging in high-dimensional, small-sample settings. In spectroscopy for planetary exploration, Laser-Induced Breakdown Spectroscopy (LIBS), Raman Spectroscopy (Raman), Visible Infrared Spectroscopy (VISIR), and Mid-Infrared Spectroscopy (MIR) each examine different aspects of composition and mineralogy, raising fundamental questions about when and how data fusion improves predictive performance. Using a Mars-relevant set of geologic standards with measurements from all four modalities, we present a rigorous systematic evaluation of four data fusion strategies: low-level (data) fusion, mid-level (feature) fusion, high-level (decision) fusion, and residual-boosting (sequential) fusion. We assess performance in predicting oxide composition via nested cross-validation and corrected significance testing to evaluate whether data fusion improves upon single-modality baselines. We show that data fusion does not uniformly improve accuracy, and that observed gains are modest, oxide-dependent, and sensitive to modality and model structure. To move beyond aggregate accuracy metrics, we use model coefficients, permutation importance, and residual gain analysis to examine how the fusion models weight individual modalities and to identify patterns of apparent complementarity or redundancy. Though focused on spectroscopy for planetary exploration, our framework for data fusion evaluation and interpretation extends to other scientific domains with heterogeneous and scarce data and provides a principled approach evaluating data fusion strategies, interpreting modality contributions, and understanding tradeoffs among data fusion strategies.

97 MATHEMATICS AND COMPUTING↗
NASA NTRS1998

First results from the aerosol lidar and backscatter sonde intercomparison campaign STRAIT'1997 at table mountain facility during February-March 1997

First results of an intercomparison measurement campaign between three aerosol lidar instruments and in-situ backscatter sondes performed at Table Mountain Facility (34.4 deg N, 117.7 deg E, 2280 m asl) in February-March 1997 are presented. During the campaign a total of 414 hours of lidar data were acquired by the Aerosol-Temperature-Lidar (ATL, Goddard Space Flight Center) the Mobile-aerosol-Raman-Lidar (MARL, Alfred Wegener Institute), and the TMF-Aerosol-Lidar (TAL, Jet Propulsion Laboratory), and four backscatter sondes were launched. From the data set altitude profiles of backscatter ratio and volume depolarization of stratospheric background aerosols at altitudes between 15 and 25 km and optically thin high-altitude cirrus clouds at altitudes below 13 km are derived. On the basis of a sulfuric acid aerosol model color ratio profiles obtained from two wavelength lidar data are compared to the corresponding profiles derived from the sonde observations. We find an excellent agreement between the in-situ and ATL lidar data with respect to backscatter and color ratio. Cirrus clouds were present on 16 of 26 nights during the campaign. Lidar observations with 17 minute temporal and 120-300 m spatial resolution indicate high spatial and temporal variability of the cirrus layers. Qualitative agreement is found between concurrent lidar measurements of backscatter ratio and volume depolarization.

Beyerle, G.↗
NASA NTRS1973

Remote measurement of atmospheric temperatures by Raman lidar.

The Raman shifted return of a lidar system has been utilized to make atmospheric temperature measurements. The measurements were made along a horizontal path at temperatures between -20 and +30 C and at ranges of about 100 meters. The temperature data were acquired by recording the intensity ratio of two portions of the rotational Raman spectrum which were simultaneously sampled from a preset range. Measurements were made to an accuracy of plus or minus 3 C with 1-minute temporal resolution.

Salzman, J. A.↗
NASA NTRS1974

Atmospheric temperature measurements, using Raman lidar

The Raman-shifted return of a lidar system had been used to make atmospheric temperature measurements. The measurements were made along a horizontal path at temperatures ranging from -30 to 30 C and at ranges of about 100 meters. The temperature data were acquired by recording the intensity ratio of two portions of the rotational Raman spectrum, which were simultaneously sampled from a preset range. These tests verified that the theoretical predictions formulated in the design of the system were adequate. Measurements were made to an accuracy of + or - 4 C with 1-minute temporal resolution.

Salzman, J. A.↗
NASA NTRS1974

Remote measurement of atmospheric temperatures by Raman lidar

The Raman shifted return of a lidar system has been utilized to make atmospheric temperature measurements. The measurements were made along a horizontal path at temperatures ranging from -30 C to +30 C and at ranges of about 100 meters. The temperature data were acquired by recording the intensity ratio of two portions of the rotational Raman spectrum which were simultaneously sampled from a preset range. A temperature measurement accuracy of plus or minus 4 C and a temporal resolution of one minute were realized with this system. The combined results of the theoretical analysis and the experimentation indicate that system improvements will significantly increase both accuracy and range.

Coney, T. A.↗