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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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At least 19 records
All sourcesNASA NTRSDOE OSTI
DOE OSTI2021

Enabling phase quantification of anhydrous cements via Raman imaging

The phase composition of Portland cements is typically determined using conventional techniques like X-ray Diffraction (XRD) Rietveld analysis, optical microscopy point counting, and electron microscopy. However, these techniques have several limitations that may affect their accuracy in certain sample-specific scenarios. Here, we report a highly accurate phase quantification of 11 different types of commercial, anhydrous cements using a new and complementary technique: Raman imaging. Specifically, for the 4 principal phases, composition from our extensive data (250,000 Raman spectra per sample, error < 0.71%) and those obtained from XRD Rietveld and supplier data have high coefficients of determination (R{sup 2} > 0.98, mean deviation <2%). Additionally, we also quantify 8 secondary phases present in cement clinkers (gypsum, anhydrite, bassanite, syngenite, dolomite, calcite, quartz, and portlandite) with a high degree of confidence, thereby demonstrating that Raman imaging is a highly versatile tool for anhydrous phase quantification in a broad variety of cements.

36 MATERIALS SCIENCE↗
NASA NTRS2020

Use of an Internal Mercury-Argon Lamp for the Calibration of Raman Frequency in Large Raman Images of Astromaterials

Raman imaging is an emerging tool for the analysis of meteorites, as it is capable of describing mineralogy, carbon composition/speciation, and crystal orientation all within a petrographic context. Adequately examining the heterogeneous composition of a meteorite, while maintaining low laser powers needed to prevent damage to meteorite mineralogy and organics, often requires the collection of large Raman images with long collection times on the timescale of days. However, the frequency calibration of the Raman instrument/spectrometer drifts on long timescales resulting in low frequency precision for the Raman spectra comprising a large Raman image. This decrease in frequency precision can compromise the analysis of geological markers that can provide important information on a meteorite sample. We examine, in detail, the change in bandwidth and frequency of the Raman bands and Hg-Ar emission lines in our Raman images as a function of time and laboratory temperature. To overcome the drift in calibration, we utilize a commercial WITec Raman instrument with an internal Hg-Ar calibration lamp to individually calibrate each spectrum in the Raman image. Our instrument, known as “Ratatoskr”, uses a beam splitter in place of the customary mirror to facilitate collection of Hg-Ar calibration lines concurrent with Raman spectra. We show that using the internal calibration we can improve the frequency precision for the spectra in our Raman images from ~±0.15 cm(exp -1) to ~±0.05 cm(exp -1) for Raman spectra collected over multiple days. This is important as it improves measurements of mineral chemistry, latent strain, and other features that are dependent upon accurate peak position determination. We also examine the spectral signal-to-noise ratio needed to minimize the frequency error when fitting bands to Gaussian/Lorentzian profiles. We then use our results to suggest a general method for calibrating the frequency of Raman spectra in large Raman images.

Jakubek, Ryan S.↗
NASA NTRSDate not supplied

Use of an Internal Mercury-Argon Lamp for the Calibration of Raman Frequency in Large Raman Images of Astromaterials

Raman imaging is an emerging tool for the analysis of meteorites, as it is capable of describing the mineralogy and organics within a petrographic context. Adequately examining the heterogeneous composition of a meteorite often requires the collection of large Raman images with long collection times on the time-scale of days. However, the frequency calibration of the Raman instrument/spectrometer drifts on long timescales resulting in low frequency precision for the Raman spectra comprising a large Raman image. Here we utilize a Hg-Ar calibration lamp integrated into our Raman microscope to calibrate the Raman spectra within a Raman image. We characterize this method of calibration in detail.

Ryan S. Jakubek↗
DOE OSTI2021

Airy light-sheet Raman imaging

Light-sheet fluorescence microscopy has greatly improved the speed and overall photostability of optically sectioning cellular and multi-cellular specimens. Similar gains have also been conferred by light-sheet Raman imaging; these schemes, however, rely on diffraction limited Gaussian beams that hinder the uniformity and size of the imaging field-of-view, and, as such, the resulting throughput rates. Here, we demonstrate that a digitally scanned Airy beam increases the Raman imaging throughput rates by more than an order of magnitude than conventional diffraction-limited beams. Overall, this, spectrometer-less, approach enabled 3D imaging of microparticles with high contrast and 1 µm axial resolution at 300 msec integration times per plane and orders of magnitude lower irradiation density than coherent Raman imaging schemes. We detail the apparatus and its performance, as well as its compatibility with fluorescence light-sheet and quantitative-phase imaging towards rapid and low phototoxicity multimodal imaging.

47 OTHER INSTRUMENTATION↗
NASA NTRS2018

Context Imaging Raman Spectrometer

Methods and systems for Raman spectroscopy and context imaging are disclosed. One or two lasers can be used to excite Raman scattering in a sample, while a plurality of LEDs can illuminate the sample at a different wavelength. The LED light is collected by a lenslet array in order to enable a high depth of field. Focusing of the image can be carried out at specific points of the image by processing the light collected by the lenslet array.

Lambert, James L.↗
DOE OSTI2021

High-fidelity and high-resolution phase mapping of granites via confocal Raman imaging

Abstract In physical sciences such as chemistry and earth sciences, specifically for characterization of minerals in a rock, automated, objective mapping methods based on elemental analysis have replaced traditional optical petrography. However, mineral phase maps obtained from these newer approaches rely on conversion of elemental compositions to mineralogical compositions and thus cannot distinguish mineral polymorphs. Secondly, these techniques often require laborious sample preparations such as sectioning, polishing, and coating which are time-consuming. Here, we develop a new Raman imaging protocol that is capable of mapping unpolished samples with an auto-focusing Z-mapping feature that allows direct fingerprinting of different polymorphs. Specifically, we report a new methodology for generating high fidelity phase maps by exploiting characteristic peak intensity ratios which can be extended to any multi-phase, heterogenous system. Collectively, these enhancements allow us to rapidly map an unpolished granite specimen (~ 2 × 2 mm) with an exceptionally high accuracy (> 97%) and an extremely fine spatial resolution (< 0.3–2 µm).

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗
DOE OSTI2024

Hyperspectral acquisition with ScanImage at the single pixel level: application to time domain coherent Raman imaging

We present a comprehensive strategy and its practical implementation using the commercial ScanImage software platform to perform hyperspectral point scanning microscopy when a fast time-dependent signal varies at each pixel level. In the proposed acquisition scheme, the scan along the X-axis is slowed down while the data acquisition is maintained at a high pace to enable the rapid acquisition of the time-dependent signal at each pixel level. The ScanImage generated raw 2D images have a very asymmetric aspect ratio between X and Y, the X axis encoding both for space and time acquisition. The results are X-axis macro-pixel where the associated time-dependent signal is sampled to provide hyperspectral information. We exemplified the proposed hyperspectral scheme in the context of time-domain coherent Raman imaging, where a pump pulse impulsively excites molecular vibrations that are subsequently probed by a time-delayed probe pulse. In this case, the time-dependent signal is a fast acousto-optics delay line that can scan a delay of 4.5ps in 25 μ s at each pixel level. With this acquisition scheme, we demonstrate ultra-fast hyperspectral vibrational imaging in the low frequency range [10 cm −1 , 150 cm −1 ] over a 500 μm field of view (64 x 64 pixels) in 130ms (∼ 7.5 frames/s). The proposed acquisition scheme can be readily extended to other applications requiring the acquisition of a fast-evolving signal at each pixel level.

Metais, Samuel↗
DOE OSTI2023

Hyperspectral Light Sheet Raman Imaging of Leaf Metabolism (Final Report)

This final technical report details the accomplishment and findings of a project that developed technology related to imaging metabolic processes in plants. The report gives technical details of the design, construction and characterization of a Raman microscope system capable of identifying chemical species using the wavelength shifts of scattered excitation light. Some of the unique aspects of the design include: use of a Bessel beam excitation source, which allow long excitation lines that are resistant to scattering in complex media such as plants; excitation at 785 nm to avoid fluorescence emission that can occur in photosynthetic organisms; and a flat optical design that makes construction and alignment significantly simpler. This project also used stable isotope labeling to look at photorespiratory flux in the leaves of three different types of plants that have different photosynthesis pathways. Gas chromatography–mass spectrometry was used to look at which metabolites and amino acids had altered oxygen, carbon and hydrogen uptake under various conditions of environmental oxygen. This generated a rich data set that is being further analyzed to understand metabolic pathways in plants. This project also used the natural fluorescence in sorghum and rice to conduct an extensive experiment across different developmental stages. Spectral differences were identified at most of the developmental stages and these can be attributed to differential pigment and pigment-protein complexes present in different relative abundances as the plant develops.

09 BIOMASS FUELS↗
DOE OSTI2023

Selective Detection in Impulsive Low-Frequency Raman Imaging Using Shaped Probe Pulses

Impulsive stimulated Raman scattering (ISRS) using a single short femtosecond pump pulse to excite molecular vibrations offers an elegant pump-probe approach to perform vibrational imaging below 200 cm –1 . One shortcoming of ISRS is its inability to offer vibrational selectivity as all the vibrational bonds whose frequencies lie within the short pump-pulse bandwidth are excited. To date, several coherent control techniques have been explored to address this issue and selectively excite a specific molecular vibration by shaping the pump pulse. There has not been any systematic work that reports an analogous shaping of the probe pulse to implement preferential detection. In this work, we focus on vibrational imaging and report vibrational selective detection by shaping the probe pulse in time. Here, we demonstrate numerically and experimentally two pulse-shaping strategies with one functioning as a vibrational notch filter and the other functioning as a vibrational low-pass filter. This enables fast (25 μs/pixel) and selective hyperspectral imaging in the low-frequency regime (< 200 cm –1 ).

74 ATOMIC AND MOLECULAR PHYSICS↗
DOE OSTI2021

Mapping Molecular Adsorption Configurations with < 5 nm Spatial Resolution through Ambient Tip-Enhanced Raman Imaging

We interrogate para-mercaptobenzoic acid (MBA) molecules chemisorbed onto plasmonic silver nanocubes through tip-enhanced Raman (TER) spectral nano-imaging. Through a detailed examination of the spectra, aided by correlation analysis and density functional theory calculations, we find that MBA chemisorbs onto the plasmonic particles with at least two distinct configurations: S- and CO2-bound. High spatial resolution TER mapping allows us to distinguish between the distinct adsorption geometries with a pixel-limited (< 5 nm) spatial resolution under ambient laboratory conditions.

Gabel, Matthew L.↗
DOE OSTI2021

A Palette of Minimally Tagged Sucrose Analogues for Real-Time Raman Imaging of Intracellular Plant Metabolism

Sucrose is the main saccharide used for longdistance transport in plants and plays an essential role in energy metabolism; however, there are no analogues for real-time imaging in live cells. We have optimised a synthetic approach to prepare sucrose analogues including very small ( 50 Da or less) Raman tags in the fructose moiety. Spectroscopic analysis identified the alkyne-tagged compound 6 as a sucrose analogue recognised by endogenous transporters in live cells and with higher Raman intensity than other sucrose derivatives. Herein, we demonstrate the application of compound 6 as the first optical probe to visualise real-time uptake and intracellular localisation of sucrose in live plant cells using Raman microscopy.

60 APPLIED LIFE SCIENCES↗
DOE OSTI2022

Correlative piezoresponse and micro-Raman imaging of CuInP 2 S 6 –In 4/3 P 2 S 6 flakes unravels phase-specific phononic fingerprint via unsupervised learning

Characterizing the novel properties of layered van der Waals materials is key for their application in functional devices. A better understanding of this type of material requires correlative imaging of diverse nanoscale material properties. Within this class of materials, CuInP 2 S 6 (CIPS) has received a significant degree of interest due to its ionically mediated room temperature ferroelectricity. Moreover, it is possible to form stable self-assembled heterostructures of ferroelectric CuInP 2 S 6 (CIPS) and non-ferroelectric (i.e., lacking Cu) In 4/3 P 2 S 6 (IPS) phases, by controlling the targeted composition and kinetics of synthesis. In this work, we present a correlative nanometric imaging study of the phononic modes and piezoelectricity of the phase-separated thin heteroepitaxial CIPS/IPS flakes. Here, we show that it is possible to isolate the different phononic modes of the two phases by spatially correlating them with their distinct ferroelectric behavior. The coupling of our experimental data with unsupervised learning statistical methods enables unraveling specific Raman peaks that are characteristic of each chemical phase (CIPS and IPS) present in the composite sample, discarding the less significant ones.

correlative microscopy↗
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↗