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DOE OSTI2020

Depth Thermography: Noninvasive 3D Temperature Profiling Using Infrared Thermal Emission

Here, we introduce a technique based on infrared thermal emission, termed depth thermography, that can remotely measure the temperature distribution beneath the surface of certain objects. Depth thermography utilizes the thermal-emission spectrum in the semitransparent spectral region of the target object to extract its temperature as a function of depth, in contrast with conventional thermography, which uses the spectrally integrated thermally emitted power to measure the surface temperature. Coupled with two-dimensional imaging, for example using an infrared hyperspectral camera or scanning a single-pixel spectrometer, this technique can yield volumetric temperature distributions. Furthermore, we carried out a proof-of-concept experiment on an asymmetrically heated fused-silica window, extracting the temperature distribution throughout the sample. Depth thermography may enable noncontact volumetric temperature measurements of microscopic objects such as multilayer electronic devices or macroscopic volumes of liquids and gases, as well as simultaneous all-optical measurements of optical and thermal properties of materials.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

NASA NTRS1990

High spatial resolution mapping of the Cepheus A region at 20, 50, and 100 microns

The Cepheus A region at 20 microns has been mapped, and a bright, unresolved central source with a peak flux of 41 Jy into a 4.0 arcsec x 4.3 arcsec beam has been detected. One-dimensional slit scans have been obtained in two perpendicular directions across Cepheus A at 50 and 100 microns using a high spatial-resolution sampling technique. The temperature and optical depth profile of the far-IR emission are determined, and a peak temperature of 46 K and peak 100 micron optical depth of 0.4 are derived. Maximum entropy deconvolution of the far-IR scans indicate that there is a bright central core with clumpy extended emission. Within errors the position of the 50/100 micron peak is the same as the 20-micron source; this is interpreted as indicating that the 20 micron radiation represents the short-wavelength emission from the core of the dust cloud seen in the far-IR. It is concluded that an embedded source provides the major source of luminosity in the Cepheus A region.

Ellis, H. B., Jr.↗

NASA NTRS1998

Aerosol analysis techniques and results from micro pulse lidar

The effect of clouds and aerosol on the atmospheric energy balance is a key global change problem. Full knowledge of aerosol distributions is difficult to obtain by passive sensing alone. Aerosol and cloud retrievals in several important areas can be significantly improved with active remote sensing by lidar. Micro Pulse Lidar (MPL) is an aerosol and cloud profilometer that provides a detailed picture of the vertical structure of boundary layer and elevated dust or smoke plume aerosols. MPL is a compact, fully eyesafe, ground-based, zenith pointing instrument capable of full-time, long-term unattended operation at 523 nm. In October of 1993, MPL began taking full-time measurements for the Atmospheric Radiation Measurement (ARM) program at its Southern Great Plains (SGP) site and has since expanded to ARM sites in the Tropical West Pacific (TWP) and the North Slope of Alaska (NSA). Other MPL's are moving out to some of the 60 world-wide Aerosol Robotic Network (AERONET) sites which are already equipped with automatic sun-sky scanning spectral radiometers providing total column optical depth measurements. Twelve additional MPL's have been purchased by NASA to add to the aerosol and cloud database of the EOS ground validation network. The original MPL vertical resolution was 300 meters but the newer versions have a vertical resolution of 30 meters. These expanding data sets offer a significant new resource for atmospheric radiation analysis. Under the direction of Jim Spinhirne, the MPL analysis team at NASA/GSFC has developed instrument correction and backscatter analysis techniques for ARM to detect cloud boundaries and analyze vertical aerosol structures. A summary of MPL applications is found in Hlavka (1997). With the aid of independent total column optical depth instruments such as the Multifilter Rotating Shadowband Radiometer (MFRSR) at the ARM sites or sun photometers at the AERONET sites, the MPL data can be calibrated, and time-resolved vertical profiles of aerosol optical depth as well as aerosol extinction can be calculated. The techniques used to calibrate the lidar, calculate the aerosol extinction-to-backscatter ratio, and produce profiles of aerosol extinction and aerosol optical depths, will be described. Results using these techniques will be presented for case studies at the ARM site in the Tropical West Pacific and later in the Southern Great Plains.

Hlavka, Dennis L.↗

DOE OSTI2023

Exploration of LIBS as a novel and rapid elemental mapping technique of nuclear fuels in the form of surrogate TRISO particles

Laser-induced breakdown spectroscopy (LIBS) was employed to characterize coatings on surrogate fuel particles. Tri-structural isotropic (TRISO) particles are a proposed nuclear fuel alternative for high temperature reactors. These particles are constructed of a ZrO 2 kernel (as a surrogate to uranium), surrounded by an inner pyrolytic carbon layer and are surrounded by an outer carbide layer (ZrC, presented here) to act as a barrier to fission products generated during nuclear reactions. These particles are embedded within a graphite compact and housed within the reactor core. Simply put, due to their robust nature, performing elemental analysis of these particles poses a challenge. Presented here, LIBS is explored as a method for characterizing elemental constituents of these particles, with the focus being on rapid elemental mapping and depth profiling. Different from traditional elemental analysis techniques (e.g., inductively coupled plasma – based methods), LIBS is advantageous because it can directly analyze the sample surface and can detect light elements such as C and O, making it a viable technique for the analysis of small, multilayered particles as spatial elemental information is warranted in the production of these particles. In the work presented here, LIBS was successfully used for discerning small layers (30–50 μm), detecting the location of carbon and oxygen layers, providing fast 2-D mapping (<5 min per particle) and rapid depth profiling (10 s per particle).

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

NASA NTRSDate not supplied

Airborne Lidar Measurements of Ozone and Aerosol Profiles Over Major US Metropolitan Areas

During field missions in 2021 and 2023, the airborne NASA Langley Research Center High Spectral Resolution Lidar 2 (HSRL 2) measured the temporal and spatial evolution of ozone and aerosol distributions impacting urban air quality over the four most populated cities in the United States. HSRL-2 measurements in 2021 were acquired over the Houston metropolitan region, including Galveston Bay and the Houston Ship Channel, as part of the NASA Tracking Aerosol Convection Experiment – Air Quality (TRACER-AQ) mission conducted in collaboration with the Department of Energy. HSRL-2 measurements were acquired over Los Angeles, Chicago, and New York City in 2023 as part of the NASA Synergistic TEMPO Air Quality Science (STAQS) mission conducted in collaboration with the NOAA Atmospheric Emissions and Reactions Observed from Megacities to Marine Areas (AEROMMA) mission. HSRL 2 provided nadir vertical profiles of ozone, aerosol backscatter, extinction, and depolarization as the aircraft flew lawnmower type patterns at 9 km for several hours over these urban areas. HSRL-2 measured profiles of aerosol extinction and aerosol optical depth (AOD) via the HSRL technique at 355 and 532 nm and profiles of aerosol backscatter and depolarization at 355, 532, and 1064 nm. Mixed Layer Heights (MLH) were derived by locating sharp vertical gradients in the profiles of aerosol backscatter. The flights were comprised of up to three repeating lawnmower patterns over each city showing the evolution of the ozone and aerosol distributions from the morning through the afternoon. The HSRL-2 measurements reveal ozone enhancements near the surface as well as in the free troposphere above the mixed layer. Some lidar measurements over Chicago and New York City show the daytime boundary layer growing into elevated layers of biomass burning aerosol. These layers complicate efforts to use column-integrated satellite measurements to infer surface air quality. As expected, mixed layer height (MLH) typically increased significantly during the day; however, during some flights, particularly over the Houston area, MLH also showed large spatial variability associated with changes in surface cover and/or small scale circulations. Often HSRL-2 measurements of AOD also showed large spatial and temporal variability throughout the day over these cities. We discuss how the ozone and aerosol profiles are averaged over different vertical and horizontal scales near the surface for use in assessments of regional air quality models and near-surface ozone retrievals from NASA’s recently launched Tropospheric Emissions: Monitoring Pollution (TEMPO) satellite.

Lidar↗

NASA NTRSDate not supplied

HSRL-2 Observations over the Houston, TX Region during TRACER-AQ

Lidar↗

DOE OSTI2024

Composition Quantification of SiGeSn Alloys Through Time-of-Flight Secondary Ion Mass Spectrometry: Calibration Methodologies and Validation With Atom Probe Tomography

Time-of-Flight Secondary Ion Mass Spectrometry (ToF-SIMS) is a powerful technique for elemental compositional analysis and depth profiling of materials. However, it encounters the problem of matrix effects that hinder its application. In this work, we introduce a pioneering ToF-SIMS calibration method tailored for SixGeySnz ternary alloys. SixGe1-x and Ge1-zSnz binary alloys with known compositions are used as calibration reference samples. Through a systematic SIMS quantification study of SiGe and GeSn binary alloys, we unveil a linear correlation between secondary ion intensity ratio and composition ratio for both SiGe and GeSn binary alloys, effectively mitigating the matrix effects. Extracted relative sensitivity factor (RSF) value from SixGe1-x (0.07 < x < 0.83) and Ge1-zSnz (0.066 < z < 0.183) binary alloys are subsequently applied to those of SixGeySnz (0.011 < x < 0.113, 0.863 < y < 0.935 and 0.023 < z < 0.103) ternary alloys for elemental compositions quantification. These values are cross-checked by Atom Probe Tomography (APT) analysis, an indication of the great accuracy and reliability of as-developed ToF-SIMS calibration process. Furthermore, the proposed method and its reference sample selection strategy in this work provide a low-cost as well as simple-to-follow calibration route for SiGeSn composition analysis, thus driving the development of next-generation multifunctional SiGeSn-related semiconductor devices.

36 MATERIALS SCIENCE↗

NASA NTRS2002

Characterization of Space Environmental Effects on Candidate Solar Sail Material

The National Aeronautics and Space Administration's (NASA) Marshall Space Flight Center (MSFC) is concentrating research into the utilization of photonic materials for spacecraft propulsion. Spacecraft propulsion, using photonic materials, will be achieved using a solar sail. A solar sail operates on the principle that photons, originating from the sun, impart pressure to the sail and therefore provide a source for spacecraft propulsion. The pressure imparted to a solar sail can be increased, up to a factor of two if the sunfacing surface is perfectly reflective. Therefore, these solar sails are generally composed of a highly reflective metallic sun-facing layer, a thin polymeric substrate and occasionally a highly emissive back surface. The Space Environmental Effects Team, at MSFC, is actively characterizing candidate solar sail material to evaluate the thermo-optical and mechanical properties after exposure to radiation environments simulating orbital environments. This paper describes the results of three candidate materials after exposure to a simulated Geosynchronous Transfer Orbit (GTO). This is the first known characterization of solar sail material exposed to space simulated radiation environments. The technique of radiation dose versus material depth profiling was used to determine the orbital equivalent exposure doses. The solar sail exposure procedures and results of the material characterization will be discussed.

Edwards, David↗

NASA NTRS2002

Characterization of Space Environmental Effects on Candidate Solar Sail Material

The National Aeronautics and Space Administration's (NASA) Marshall Space Flight Center (MSFC) is concentrating research into the utilization of photonic materials for spacecraft propulsion. Spacecraft propulsion, using photonic materials, will be achieved using a solar sail. A sail operates on the principle that photons, originating from the sun, impart pressure and provide a source of spacecraft propulsion. The pressure can be increased, by a factor of two if the sun-facing surface is perfectly reflective. Solar sails are generally composed of a highly reflective metallic front layer, a thin polymeric substrate, and occasionally a highly emissive back surface. The Space Environmental Effects Team at MSFC is actively characterizing candidate solar sail materials to evaluate the thermo-optical and mechanical properties after exposure to a simulated Geosynchronous Transfer Orbit (GTO) radiation environment. The technique of radiation dose verses material depth profiling was used to determine the orbital equivalent exposure doses. The solar sail exposure procedures and results of the material characterization will be discussed.

Edwards, David↗

NASA NTRSDate not supplied

Evaluating Combined Lidar and Polarimeter Measurements of Cloud Top Parameters (Extinction, Scattering Cross Sections, and Droplet Number Density, Liquid Water Content)

We present a new method to derive profiles of extinction from a lidar which is then combined with polarimeter measurements to derive cloud droplet number density (CDNC) in the tops of warm clouds. The method employs polarization-sensitive elastic backscatter lidar measurements to estimate attenuation of the lidar signal within the cloud and polarimeter estimates of cloud droplet size distributions. The measurements used for this demonstration are from NASA Langley Research Center’s High Spectral Resolution Lidar – Generation 2 (HSRL-2) and NASA GISS’s Research Scanning Polarimeter (RSP). The measurements were acquired on NASA’s ACTIVATE mission, during which the instruments were deployed in a down-looking mode from a high-altitude aircraft, which flew in coordination with a low-flying aircraft acquiring coincident in situ measurements of cloud droplet size and number. The high vertical (1.25 m) and horizontal (~50 m) sampling resolution of the HSRL-2 data enabled retrievals of single-scattering extinction profiles to within ~2.5 optical depths of cloud top. Another key feature of the method was the well-calibrated measurement of backscatter at cloud top due to using the HSRL technique. The RSP retrievals of cloud droplet effective radius and variance were accomplished using the “cloud-bow” technique. Overall, the technique provides extinction profile estimates for the top 2.5 optical depths of water clouds that can be used to estimate the cloud droplet number density in various types of warm clouds. The mean extinction values at cloud top (0-1 optical depth) are compared against cloud drop size and number concentration acquired from wing-mounted probes (e.g., DMT Cloud Droplet Probe - CDP, SPEC Fast Cloud Droplet Probe FCDP, and SPEC 2D Stereo Probe - 2DS) that were deployed on the low-flying aircraft. Comparisons between the effective radius and variance from the polarimeter, lidar ratio (extinction to backscatter) from the lidar and polarimeter, and LWC are also presented. All measurements were acquired over the Western North Atlantic over 3 years from 2020 to 2022.

lidar↗

NASA NTRS1993

Depth-diameter ratios for Martian impact craters: Implications for target properties and episodes of degradation

This study determines crater depth through use of photoclinometric profiles. Random checks of the photoclinometric results are performed using shadow estimation techniques. The images are Viking Orbiter digital format frames; in cases where the digital image is unusable for photoclinometric analysis, shadow estimation is used to determine crater depths. The two techniques provide depth results within 2 percent of each other. Crater diameters are obtained from the photoclinometric profiles and checked against the diameters measured from the hard-copy images using a digitizer. All images used in this analysis are of approximately 40 m/pixel resolution. The sites that have been analyzed to date include areas within Arabia, Maja Valles, Memnonia, Acidalia, and Elysium. Only results for simple craters (craters less than 5 km in diameter) are discussed here because of the low numbers of complex craters presently measured in the analysis. General results indicate that impact craters are deeper than average. A single d/D relationship for fresh impact craters on Mars does not exist due to changes in target properties across the planet's surface. Within regions where target properties are approximately constant, however, d/D ratios for fresh craters can be determined. In these regions, the d/D ratios of nonpristine craters can be compared with the fresh crater d/D relationship to obtain information on relative degrees of crater degradation. This technique reveals that regional episodes of enhanced degradation have occurred. However, the lack of statistically reliable size-frequency distribution data prevents comparison of the relative ages of these events between different regions, and thus determination of a large-scale episode (or perhaps several episodes) cannot be made at this time.

Barlow, N. G.↗

DOE OSTI2020

Understanding Measurement Artifacts Causing Inherent Cation Gradients in Depth Profiles of Perovskite Photovoltaics with TOF-SIMS

Time-of-flight secondary-ion mass spectrometry (TOF-SIMS) is one of the few techniques that can obtain chemical information from the hybrid organic-inorganic perovskite solar cells (PSCs) in one dimension (standard depth profiling), two dimensions (high-resolution 100-nm imaging), as well as three dimensions (tomography combining high-resolution imaging with depth profiling). We have very recently developed thermo-mechanical methods to cleave perovskite samples at the back transparent conducting oxide/PSC interface. This allowed for depth-profiling from the back of the device to the front. The resultant profiles answered the lingering question of the apparent A-site cation gradient typically seen in TOF-SIMS depth profiles. In fact, this gradient is a measurement artifact due to beam damage that the community should be informed of as TOF-SIMS data become more commonly employed. Methods of mitigating this artifact by altering the measurement conditions are also presented.

14 SOLAR ENERGY↗

NASA NTRS1972

Profiling with the electron microscope.

Discussion of a profiling technique using a scanning electron microscope for obtaining depth information on a single micrograph of a small specimen. A stationary electron beam is used to form a series of contamination spots in a line across the specimen. Micrographs obtained by this technique are useful as a means of projection and display where stereo viewers are not practical.

Vedder, J. F.↗

NASA NTRS2002

Detection of Intergranular Corrosion in Cold Plate Face Sheets

Cold plates are critical for cooling electronic systems in the shuttle. As a result of the environmental conditions in which they operate, water can condense between them and a support shelf. In some cases, this water results in intergranular corrosion in the face sheet. If the intergranular corrosion sufficiently penetrates the face sheet, a coolant leak could occur and jeopardize cold plate operation. This paper examines techniques for detecting and characterizing the intergranular corrosion, to enable recertification of cold plates that have been in operation for 15 plus years. Intergranular corrosion was artificially induced in the face sheets of a series of cold plate specimens using an electrochemical process. Some of the cold plate specimens were separated for destructive characterization of the extent of corrosion produced by the electrochemical process and to insure the induced corrosion was intergranular. The rest of the specimens were characterized nondestructively using several techniques. X-ray tomography and ultrasonic techniques provided the best indication of corrosion in these specimens and will be the focus of this paper. An x-ray tomography technique was shown to be the most effective technique for characterizing depth of the intergranular corrosion. From these measurements, corrosion profile maps were developed that were consistent with subsequent destructive evaluations of the specimens. This enabled the assessment of NDE (ondestructive evaluation) standards to evaluate the viability of other NDE techniques. Due to system constraints, a different technique must be used to inspect an entire cold plate. An ultrasonic technique was shown to be very reliable for detection of corrosion in the unbacked regions of the face sheet. The ultrasonic technique was performed in an alcohol bath to avoid additional corrosion during the NDE evaluation. A pulse echo technique that focuses on the RMS value of the signal is shown to be very sensitive to the presence of intergranular corrosion.

Winfree, William P.↗

NASA NTRS1974

Identification characteristics of certain lunar relief forms on pictures obtained from spacecraft

This investigation was restricted to the determination of recognitional characteristics of a single type of relief form, dimple craters on the surface of maria. These craters were arbitrarily considered as closed, negative relief forms, circular in plan-view, and symmetric relative to the center. Two techniques were used to determine the shadow configuration in the craters: (1) experimental determination of the shadow edge by illuminating the models of different profile shapes with a parallel light beam; and (2) geometric construction of the shadow edge using a vertical section of the formation in the direction of the solar rays. A morphological map of the surface which includes the following factors can be compiled using the proposed identification technique: crater profile nature, crater diameter, ratio of diameter and depth, sharpness of the lip, and distribution density of the forms.

Kravtsova, V. I.↗

DOE OSTI2020

In-Depth Mass Spectrometry-Based Single-Cell and Nanoscale Proteomics

Leukemic stem cells are highly dynamic and heterogeneous. Analysis of leukemic stem cells at the single cell level should provide a wealth of insights that would not be possible using bulk measurements. Mass spectrometry (MS)-based proteomic workflows can quantify hundreds or thousands of proteins from a biological sample and has proven invaluable for biomedical research, but samples comprising large numbers of cells are typically required due to limited sensitivity. Recent developments in sample processing, chromatographic separations and MS instrumentation are now extending in-depth proteome profiling to single mammalian cells. We describe specific techniques that increase the sensitivity of single-cell proteomics by orders of magnitude, enabling the promise of single cell proteomics to become a reality. We anticipate such techniques could significantly advance our understanding of leukemic stem cells.

Liang, Yiran↗

NASA NTRS1979

Measurement techniques for trace metals in coal-plant effluents: A brief review

The strong features and limitations of techniques for determining trace elements in aerosols emitted from coal plants are discussed. Techniques reviewed include atomic absorption spectroscopy, charged particle scattering and activation, instrumental neutron activation analysis, gas/liquid chromatography, gas chromatographic/mass spectrometric methods, X-ray fluorescence, and charged-particle-induced X-ray emission. The latter two methods are emphasized. They provide simultaneous, sensitive multielement analyses and lend themselves readily to depth profiling. It is recommended that whenever feasible, two or more complementary techniques should be used for analyzing environmental samples.

Singh, J. J.↗

DOE OSTI2025

Estimating Soil Thermal Inertia Profiles From the Passive Equilibration of a Temperature Probe

Knowledge of the distribution of soil thermal properties is important for understanding subsurface hydrological and biogeochemical processes. This study describes and evaluates quick thermal profiling (QTP), a new measurement technique aimed at providing rapid, depth-resolved measurements of soil thermal inertia at numerous locations across the landscape. A cylindrical probe with temperature sensors at multiple depths is quickly inserted into the ground, and soil thermal inertia is estimated from how quickly the probe temperature equilibrates with the soil. To this end, a finite volume heat transfer model is used to generate temperature equilibration time series across combinations of controlling factors, and a gridded search inversion approach is applied to infer soil thermal inertia. Field tests in the Arctic indicate that QTP measurements have a minimum uncertainty of 0.14 J m −2 K −1 s −1/2 and covary with dual-probe heat pulse thermal analyzer measurements (concordance correlation coefficient = 0.56) with a root-mean-square error of 0.40 J m −2 K −1 s −1/2 . Besides demonstrating the value of QTP for estimating thermal inertia, this study identifies various sources of measurement uncertainty, particularly probe-soil contact resistance and frictional heating. Further, analysis of soil samples indicates that thermal inertia can be used to estimate thermal conductivity and dry bulk density in the studied area, although such inferences are highly site-specific. Overall, the QTP method holds promise to generate thermal inertia data products and to complement other characterization approaches for advancing understanding of soil properties across far more locations than is currently possible.

Lamb, J. R. [Lawrence Berkeley National Laboratory↗