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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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Portable Electron Microscopy for ISS and Beyond
Advances in space exploration have evolved in lockstep with key technology advances in diverse fields such as materials science, biological science, and engineering risk management. Research in these areas, where structure and physical processes come together, can proceed rapidly in part due to sophisticated ground-based analytical tools that help re-searchers develop technologies and engineering processes that push frontiers of human space exploration. Electron microscopes (EM) are an example of such a workhorse tool, lending a unique blend of strong optical scattering, high native resolution, large depth of focus, and spectroscopy via characteristic X-ray emission, providing exquisite high-magnification structural imaging and chemical analysis. Ground-based EM’s have been essential in NASA research for many years. In particular, in mineralogy and petrology, EM is used to understand the origin and evolution of the solar system, particularly rocky bodies. In microbiology, EM has helped visualize the architecture of tissues and cells. In engineering/materials science, EM has been used to characterize particulate debris in air and water samples, determine pore sizes in ceramics/catalysts, understand the nature of fibers, determine composition and morphology of new and existing materials, and characterize micro-textures of vapor deposited films. EM is highly effective at investigating a wide variety of nanoscale materials/biomaterials at the core of many of NASA’s inquiries. Despite exquisite optical performance and versatility, EM’s are traditionally large, heavy, and have high power consumption. They are also expensive so they tend to be housed at universities and large research institutions, or at major industrial laboratory sites with support staff, supplies, and skilled operators. Since most organizations cannot support their own EM, samples are often sent to these large institutions and service centers to be imaged, at great expense and of-ten with delay of weeks to months for complex analyses. Complexity, high cost, and maintenance associated with collecting EM image data has until now severely limited fields in which EM is used. Making EM accessible outside constrained terrestrial laboratory environments will bring EM’s performance and versatility to a much broader range of scientific and engineering endeavors, including in space.
Portable Flow Device Using Fourier Ptychography Microscopy and Deep Learning for Detection of Biosignatures
A proof-of-concept, compact, portable Fourier Ptychographic Microscope (FPM) to perform wide field-of-view, high spatial resolution imaging (<1 μm) for biosignature motility in liquid samples, is presented. The FPM has the potential to be developed as a space-based payload for future landers destined to the Ocean Worlds. A portable FPM using an existing Fourier ptychography (FP) algorithm adapted for reconstruction is demonstrated. A NVIDIA Jetson Nano board and camera combined with FP, is used to computationally reconstruct sub-micron resolution images. Additionally, deep learning was employed to perform inferencing prediction which enables the on-edge FPM device.
Below Band-Gap Laser Ablation of Diamond for Transmission Electron Microscopy
A 248-nm excimer laser was used to thin naturally occurring type 1a diamond substrates at normal and glancing (22 deg) incidence. Perforation of a 250 micron thick substrate was achieved in about 15 minutes at normal incidence. Whilst the substrate thinned at glancing incidence was found to have large electron-transparent areas, that thinned at normal incidence required additional argon milling to achieve electron transparency. X-ray photoelectron spectroscopy of the back surface of the diamond failed to detect any graphite or glassy carbon, confirming that damage due to laser ablation occurs only at the incident surface. Samples prepared using this technique imaged in the transmission electron microscope were observed to have retained the nitrogen platelets
A Correlative Electron Microscopy Study of a Ru-rich Metal Grain from a Calcium-aluminum-rich Inclusion
Calcium-aluminum-rich inclusions (CAIs) are sub-mm to cm-sized objects composed of highly refractory Ca- and Al-rich mineral phases, hosted in chondritic meteorites. The component minerals of CAIs were thermodynamically predicted to be condense at high temperatures in the cooling solar nebula. Isotopic analyses place the age of these objects at 4.567 Ga, making them the first formed solids in our solar system. The chemical compositions and crystal structures of the Ca- and Al-rich minerals serve as imprints of the thermochemical environments in which they formed. Therefore, detailed microstructural analyses of CAIs can provide insight into the processes that prevailed in the early solar system.
Validation of Crystal Plasticity Simulations Using High Energy X-ray Diffraction Microscopy Measurements
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Investigating Space Weathering of Ryugu Grains Using Electron Microscopy and X-Ray Computed Tomography
The effects of micrometeorite bombardment and solar wind ion irradiation – collectively known as space weathering – alter the microstructural, chemical, and spectral properties of airless surfaces. Characteristics of space weathering include vesiculated textures, amorphous grain rims (upper ~100 nm), and the production of Fe-bearing nanoparticles (npFe). The resulting modifications in the optical properties of the surface regolith include changes in spectral slope and overall reflectance of the surfaces as well as the attenuation of their characteristic absorption bands across VIS-NIR wavelengths. As the surface is continuously exposed to interplanetary space over time, the accrual of these features complicates the interpretation of remote sensing spectral data and the characterization of returned samples. Laboratory experiments that simulate solar wind irradiation and micrometeoroid impacts using carbonaceous analogs have revealed novel and complex microstructural and chemical changes, including the decrease in organic species concentrations and the reduction of Fe 3+ . In 2020, the Japan Aerospace Exploration Agency (JAXA)’s Hayabusa2 mission returned over 5 g of regolith particles from near- Earth C-type asteroid (162173) Ryugu – a unique opportunity to study space weathering on carbonaceous materials. Initial studies have established that the surface morphology and chemical signatures of space weathering in returned samples share characteristics with laser irradiation experiments simulating micrometeoroid bombardment, indicating that impacts are a significant space weathering mechanism operating on Ryugu. Here, we seek to improve our understanding of space weathering of carbonaceous asteroidal regolith grains by characterizing its effects directly on returned samples to determine the nature of space weathering on Ryugu. To do so, we performed coordinated analyses using electron beam techniques and X-ray computed tomography (XCT) to examine the effects of space weathering on grains returned from the surface of Ryugu by the Hayabusa2 mission.
Electron Microscopy of Microbial Biomass
As humans move to long term stays in space their microbes move with them. This poses problems as the microbes can colonize various life support systems, creating biofilms that can grow and spread, which in turn causes obstructions and ultimately degrades function of these systems. MSFC currently has no protocol in place for the Scanning Electron Microscope (SEM) imaging of microbes.
Extended depth-of-field light-sheet microscopy improves imaging of large volumes at high numerical aperture
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Two-Photon Fluorescence Microscope for Microgravity Research
A two-photon fluorescence microscope has been developed for the study of biophysical phenomena. Two-photon microscopy is a novel form of laser-based scanning microscopy that enables three-dimensional imaging without many of the problems inherent in confocal microscopy. Unlike one-photon optical microscopy, two-photon microscopy utilizes the simultaneous nonlinear absorption of two near-infrared photons. However, the efficiency of two-photon absorption is much lower than that of one-photon absorption, so an ultra-fast pulsed laser source is typically employed. On the other hand, the critical energy threshold for two-photon absorption leads to fluorophore excitation that is intrinsically localized to the focal volume. Consequently, two-photon microscopy enables optical sectioning and confocal performance without the need for a signal-limiting pinhole. In addition, there is a reduction (relative to one-photon optical microscopy) in photon-induced damage because of the longer excitation wavelength. This reduction is especially advantageous for in vivo studies. Relative to confocal microscopy, there is also a reduction in background fluorescence, and, because of a reduction in Rayleigh scattering, there is a 4 increase of penetration depth. The prohibitive cost of a commercial two-photon fluorescence-microscope system, as well as a need for modularity, has led to the construction of a custom-built system (see Figure 1). This system includes a coherent mode-locked titanium: sapphire laser emitting 120-fs-duration pulses at a repetition rate of 80 MHz. The pulsed laser has an average output power of 800 mW and a wavelength tuning range of 700 to 980 nm, enabling the excitation of a variety of targeted fluorophores. The output from the laser is attenuated, spatially filtered, and then directed into a confocal scanning head that has been modified to provide for side entry of the laser beam. The laser output coupler has been replaced with a dichroic filter that reflects the longer-wavelength excitation light and passes the shorter-wavelength fluorescence light. Also, the confocal pinhole has been removed to increase the signal strength. The laser beam is scanned by a twoperpendicular- axis pair of galvanometer mirrors through a pupil transfer lens into the side port of an inverted microscope. Finally, the beam is focused by a 63-magnification, 1.3-numerical- aperture oil-immersion objective lens onto a specimen. The pupil transfer lens serves to match the intermediate image planes of the scanning head and the microscope, and its location is critical. In order to maximize the quality of the image, (that is, the point spread function of the objective lens for all scan positions), the entire system was modeled in optical-design software, and the various free design parameters (the parameters of the spatial-filter components as well as the separations of all of the system components) were determined through an iterative optimization process. A modular design was chosen to facilitate access to the optical train for future fluorescence correlation spectroscopy and fluorescence-lifetime experiments.
Lunar resources: Oxygen from rocks and soil
The first set of hydrogen reduction experiments to use actual lunar material was recently completed. The sample, 70035, is a coarse-grained vesicular basalt containing 18.46 wt. percent FeO and 12.97 wt. percent TiO2. The mineralogy includes pyroxene, ilmenite, plagioclase, and minor olivine. The sample was crushed to a grain size of less than 500 microns. The crushed basalt was reduced with hydrogen in seven tests at temperatures of 900-1050 C and pressures of 1-10 atm for 30-60 minutes. A capacitance probe, measuring the dew point of the gas stream, was used to follow reaction progress. Experiments were also conducted using a terrestrial basalt similar to some lunar mare samples. Minnesota Lunar Simulant (MLS-1) contains 13.29 wt. percent FeO, 2.96 wt. percent Fe2O3, and 6.56 wt. percent TiO2. The major minerals include plagioclase, pyroxene, olivine, ilmenite, and magnetite. The rock was ground and seived, and experiments were run on the less than 74- and 500-1168-micron fractions. Experiments were also conducted on less than 74-micron powders of olivine, pyroxene, synthetic ilmenite, and TiO2. The terrestrial rock and mineral samples were reduced with flowing hydrogen at 1100 C in a microbalance furnace, with reaction progress monitored by weight loss. Experiments were run at atmospheric pressure for durations of 3-4 hr. Solid samples from both sets of experiments were analyzed by Mossbauer spectroscopy, petrographic microscopy, scanning electron microscopy, tunneling electron microscopy, and x-ray diffraction. Apollo 17 soil 78221 was examined for evidence of natural reduction in the lunar environment. This sample was chosen based on its high maturity level (I sub s/FeO = 93.0). The FeO content is 11.68 wt. percent and the TiO2 content is 3.84 wt. percent. A polished thin section of the 90-150 micron size fraction was analyzed by petrographic microscopy and scanning electron microscopy.
Soil Analysis Micro-Mission Concepts Derived from the MSP 2001 Mars Environmental Compatibility Assessment (MECA)
The Mars Environmental Compatibility Assessment (MECA) will evaluate the Martian environment for soil and dust-related hazards to human exploration as part of the Mars Surveyor Program 2001 Lander. The integrated MECA payload contains a wet-chemistry laboratory, a microscopy station, an electrometer to characterize the electrostatic environment, and arrays of material patches to study abrasion and adhesion. Heritage will be all-important for low cost micro-missions, and adaptations of instruments developed for the Pathfinder, '98 and '01 Landers should be strong contenders for '03 flights. This talk has three objectives: (1) Familiarize the audience with MECA instrument capabilities; (2) present concepts for stand-alone and/or mobile versions of MECA instruments; and (3) broaden the context of the MECA instruments from human exploration to a comprehensive scientific survey of Mars. Due to time limitations, emphasis will be on the chemistry and microscopy experiments. Ion-selective electrodes and related sensors in MECA's wet-chemistry laboratory will evaluate total dissolved solids, redox potential, pH, and the concentration of many soluble ions and gases in wet Martian soil. These electrodes can detect potentially dangerous heavy-metal ions, emitted pathogenic gases, and the soil's corrosive potential, and experiments will include cyclic voltammetry and anodic stripping. For experiments beyond 2001, enhancements could allow multiple use of the cells (for mobile experiments) and reagent addition (for quantitative mineralogical and exobiological analysis). MECA's microscopy station combines optical and atomic-force microscopy (AFM) in an actively focused, controlled illumination environment to image particles from millimeters to nanometers in size. Careful selection of substrates allows controlled experiments in adhesion, abrasion, hardness, aggregation, magnetic and other properties. Special tools allow primitive manipulation (brushing and scraping) of samples. Soil particle properties including size, shape, color, hardness, adhesive potential (electrostatic and magnetic), will be determined using an array of sample receptacles and collection substrates. The simple, rugged atomic-force microscope will image in the submicron size range and has the capability of performing a particle-by-particle analysis of the dust and soil. Future implementations might enhance the optical microscopy with spectroscopy, or incorporate advanced AFM techniques for thermogravimetric and chemical analysis.
Nondestructive evaluation of structural ceramics
A review is presented on research and development of techniques for nondestructive evaluation and characterization of advanced ceramics for heat engine applications. Highlighted in this review are Lewis Research Center efforts in microfocus radiography, scanning laser acoustic microscopy (SLAM), scanning acoustic microscopy (SAM), scanning electron acoustic microscopy (SEAM), and photoacoustic microscopy (PAM). The techniques were evaluated by applying them to research samples of green and sintered silicon nitride and silicon carbide in the form of modulus-of-rupture bars containing seeded voids. Probabilities of detection of voids were determined for diameters as small as 20 microns for microfucus radiography, SLAM, and SAM. Strengths and limitations of the techniques for ceramic applications are identified. Application of ultrasonics for characterizing ceramic microstructures is also discussed.
Ultrasonic NDE of structural ceramics for power and propulsion systems
A review of research investigations of several ultrasonic evaluation techniques applicable to structural ceramics for advanced heat engines is presented. This review highlights recent work conducted under the sponsorship of and at the Lewis Research Center. Results obtained with scanning acoustic microscopy, scanning laser acoustic microscopy, photo acoustic microscopy, and scanning electron acoustic microscopy are compared. In addition to these flaw imaging techniques, microstructure characterization by analytical ultrasonics is described. The techniques were evaluated by application to research samples of monolithic silicon nitride and silicon carbide in the form of discs and bars containing naturally occurring and deliberately-introduced flaws and microstructural anomalies. Strengths and limitations of the techniques are discussed.
Nondestructive evaluation of sintered ceramics
Radiography and several acoustic and thermoacoustic microscopy techniques are investigated for application to structural ceramics for advanced heat engines. A comparison is made of the results obtained from the use of scanning acoustic microscopy (SAM), scanning laser acoustic microscopy (SLAM), and thermoacoustic microscopy (TAM). These techniques are evaluated on research samples of green and sintered monolithic silicon nitrides and silicon carbides in the form of modulus-of-rupture (MOR) bars containing deliberately introduced flaws. Strengths and limitations of the techniques are described, with the emphasis being on statistics of detectability of flaws that constitute potential fracture origins. Further, it is shown that radiographic evaluation and guidance helped develop uniform high-density Si3N4 MOR bars with improved four-point flexural strength (875, 544, and 462 MPa at room temperature, 1200 C, 1370 C, respectively) and reduced scatter in bend strength.
Morphological studies of bone and tendon
The Soviet biosatellite Cosmos 2044 carried adult rats on a spaceflight that lasted 13.8 days and was intended to repeat animal studies carrier out on Cosmos 1887. Skeletal tissue and tendon from animals flown on Cosmos 2044 were studied by light and electron microscopy, histochemistry, and morphometric techniques. Studies were confined to the bone cells and vasculature from the weight-bearing tibias. Results indicated that vascular changes at the periosteal and subperiosteal region of the tibia were not apparent by light microscopy or histochemistry. However, electron microscopy indicated that vascular influsions were present in bone samples from the flight animals. A unique combination of microscopy and histochemical techniques indicated that the endosteal osteoblasts from this same middiaphyseal region demonstrated a slight (but not statisticallly significant) reduction in bone cell activity. Electron-microscopic studies of the tendons from metatarsal bones showed a collagen fibril disorganization as a result of spaceflight. Thus changes described for Cosmos 1887 were present in Cosmos 2044, but the changes ascribed to spaceflight were not as evident.