Search NASA⌕ Search

SEARCH · Search NASA

Results for “microscopy analysis”

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.

Quote a phrase for an exact phrase match. Source license links do not imply unrestricted reuse.

At least 19 records

Scanning Tunneling Microscopy analysis of space-exposed polymer films

The characterization of the surface of selected space-exposed polymer films by Scanning Tunneling Microscopy (STM) is reported. Principles of STM, an emerging new technique for materials analysis, are reviewed. The analysis of several films which received up to 5.8 years of low Earth orbital (LEO) exposure onboard the NASA Long Duration Exposure Facility (LDEF) is discussed. Specimens included FEP Teflon thermal blanket material, Kapton film, and several experimental polymer films. Ultraviolet and atomic oxygen-induced crazing and erosion are described. The intent of this paper is to demonstrate how STM is enhancing the understanding of LEO space environmental effects on polymer films.

Kalil, Carol R.↗

Electron Microscopy Abrasion Analysis of Candidate Fabrics for Planetary Space Suit Protective Overgarment Application

The Electron Microscopy Abrasion Analysis of Candidate Fabrics for Planetary Space Suit Protective Overgarment Application is in support of the Abrasion Resistance Materials Screening Test. The fundamental assumption made for the SEM abrasion analysis was that woven fabrics to be used as the outermost layer of the protective overgarment in the design of the future, planetary space suits perform best when new. It is the goal of this study to determine which of the candidate fabrics was abraded the least in the tumble test. The sample that was abraded the least will be identified at the end of the report as the primary candidate fabric for further investigation. In addition, this analysis will determine if the abrasion seen by the laboratory tumbled samples is representative of actual EVA Apollo abrasion.

Hennessy, Mary J.↗

Tutorial on In Situ and Operando (Scanning) Transmission Electron Microscopy for Analysis of Nanoscale Structure–Property Relationships

In situ and operando (scanning) transmission electron microscopy [(S)TEM] is a powerful characterization technique that uses imaging, diffraction, and spectroscopy to gain nano-to-atomic scale insights into the structure–property relationships in materials. This technique is both customizable and complex because many factors impact the ability to collect structural, compositional, and bonding information from a sample during environmental exposure or under application of an external stimulus. In the past two decades, in situ and operando (S)TEM methods have diversified and grown to encompass additional capabilities, higher degrees of precision, dynamic tracking abilities, enhanced reproducibility, and improved analytical tools. Much of this growth has been shared through the community and within commercialized products that enable rapid adoption and training in this approach. This tutorial aims to serve as a guide for students, collaborators, and nonspecialists to learn the important factors that impact the success of in situ and operando (S)TEM experiments and assess the value of the results obtained. As this is not a step-by-step guide, readers are encouraged to seek out the many comprehensive resources available for gaining a deeper understanding of in situ and operando (S)TEM methods, property measurements, data acquisition, reproducibility, and data analytics.

(S)TEM↗

Advanced hydrogen electrode for hydrogen-bromide battery

Binary platinum alloys are being developed as hydrogen electrocatalysts for use in a hydrogen bromide battery system. These alloys were varied in terms of alloy component mole ratio and heat treatment temperature. Electrocatalyst evaluation, performed in the absence and presence of bromide ion, includes floating half cell polarization studies, electrochemical surface area measurements, X ray diffraction analysis, scanning electron microscopy analysis and corrosion measurements. Results obtained to date indicate a platinum rich alloy has the best tolerance to bromide ion poisoning.

Kosek, Jack A.↗

Physics-based reward driven image analysis in microscopy

The rise of electron microscopy has expanded our ability to acquire nanometer and atomically resolved images of complex materials. The resulting vast datasets are typically analyzed by human operators, an intrinsically challenging process due to the multiple possible analysis steps and the corresponding need to build and optimize complex analysis workflows. We present a methodology based on the concept of a Reward Function coupled with Bayesian Optimization, to optimize image analysis workflows dynamically. The Reward Function is engineered to closely align with the experimental objectives and broader context and is quantifiable upon completion of the analysis. Here, cross-section, high-angle annular dark field (HAADF) images of ion-irradiated (Y, Dy)Ba 2 Cu 3 O 7–δ thin-films were used as a model system. The reward functions were formed based on the expected materials density and atomic spacings and used to drive multi-objective optimization of the classical Laplacian-of-Gaussian (LoG) method. These results can be benchmarked against the DCNN segmentation. This optimized LoG* compares favorably against DCNN in the presence of the additional noise. We further extend the reward function approach towards the identification of partially-disordered regions, creating a physics-driven reward function and action space of high-dimensional clustering. We pose that with correct definition, the reward function approach allows real-time optimization of complex analysis workflows at much higher speeds and lower computational costs than classical DCNN-based inference, ensuring the attainment of results that are both precise and aligned with the human-defined objectives.

47 OTHER INSTRUMENTATION↗

High temperature deformation of hot-pressed polycrystalline orthoenstatite

Artificial hot pressed polycrystalline samples were prepared from purified powder of Bamble, Norway, orthoenstatite, (Mg0.86Fe0.14)SiO3. The uniaxial creep behavior of the polycrystalline orthoenstatite was studied over stress ranges of 10-180 MPa and temperatures of 1500-1700 K (0.82-0.93 T sub m) under two different oxygen fugacities, namely equilibrium (Mo-MoO2 buffer) and a reducing (graphite heating element) atmosphere, respectively. An intergranular glassy phase of different compositions with a cavitational creep deformation were observed. In the Mo-MoO2 buffer atmosphere with PO2 approx. 10 to the minus 11 power - 10 to the minus 13 power atmospheres, the results of an analytical electron microscopy analysis indicate that the glassy phases are richer in Ca and Al due to the residual impurities after hot pressing. In the reducing atmosphere with an oxygen fugacity of PO2 approx. 10 to the minus 3 power - 10 to the minus 25 power atmospheres, the results of analytical electron microscopy analysis indicate that the glassy phase is almost pure silica with the presence of free iron precipitate on grain facets and at triple junctions due to the reduction of bulk materials.

Dehghan-Banadaki, A.↗

Effect of molecular permanent dipole moment on guest aggregation and exciton quenching in phosphorescent organic light emitting diodes

This study explores the effect of molecular permanent dipole moment (PDM) on aggregation of guest molecules in phosphorescent host–guest organic light-emitting diodes (OLEDs). Through a combination of photoluminescence measurements, high-angle annular dark-field scanning transmission electron microscopy analysis, and an Ising model based physical vapor-deposition simulation, we show that higher PDM of tris[2-phenylpyridinato-C2,N]iridium(III) guest can actually lead to a reduced aggregation relative to tris[bis[2-(2-pyridinyl-N)phenyl-C] (acetylacetonato)iridium(III) when doped into a non-polar host 1,3,5-tris(carbazol-9-yl)benzene. This study further explores the effect of host polarity by using a polar host 3′,5′-di(carbazol-9-yl)-[1,1′-biphenyl]-3,5-dicarbonitrile, and it is shown that the polar host leads to reduced guest aggregation. In conclusion, this study provides a comprehensive understanding of the impact of molecular PDM on OLED material efficiency and stability, providing insights for optimizing phosphorescent OLED materials.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Ion velocity effect governs damage annealing process in defective KTaO 3

Effects of electronic to nuclear energy losses (S e /S n ) ratio on damage evolution in defective KTaO 3 have been investigated by irradiating pre-damaged single crystal KTaO 3 with intermediate energy O ions (6 MeV, 8 MeV and 12 MeV) at 300 K. By exploring these processes in pre-damaged KTaO 3 containing a fractional disorder level of 0.35, the results demonstrate the occurrence of a precursory stage of damage production before the onset of damage annealing process in defective KTaO 3 that decreases with O ion energy. The observed ionization-induced annealing process by ion channeling analysis has been further mirrored by high resolution transmission electron microscopy analysis. In addition, the reduction of disorder level is accompanied by the broadening of the disorder profiles to greater depth with increasing ion fluence, and enhanced migration is observed with decreasing O ion energy. Since S e (~3.0 keV nm –1 ) is nearly constant for all 3 ion energies across the pre-damaged depth, the difference in behavior is due to the so-called 'velocity effect': the lower ion velocity below the Bragg peak yields a confined spread of the electron cascade and hence an increased energy deposition density. Here, the inelastic thermal spike calculation has further confirmed the existence of a velocity effect, not previously reported in KTaO 3 or very scarcely reported in other materials for which the existence of ionization-induced annealing has been reported. In other words, understanding of ionization-induced annealing has been advanced by pointing out that ion velocity effect governs the healing of pre-existing defects, which may have significant implication for the creation of new functionalities in KTaO 3 through atomic-level control of microstructural modifications, but may not be limited to KTaO 3 .

74 ATOMIC AND MOLECULAR PHYSICS↗

Chemical, Structural, and Microstructural Changes in Metallic and Silicon-Based Coating Materials Exposed to Iodine Vapor

The chemical, structural and microstructural behavior of steels (304, 316 and A36), titanium-aluminum alloy (Ti-Al, (6Al-4V)), aluminum-magnesium alloy (Al-Mg, 6061), and coatings (Silcolloy and Dursan (SilcoTek Corporation)) were probed after exposure to iodine laminar flow. Exposures were carried out in a custom-built Iodine Vapor RIG (IVR) at 300 degrees C to an iodine laminar vapor flow of 1 mg min(exp. -1), carried by 145 mL-min(exp. -1) argon gas, for 5, 15 and 30 days. Samples were characterized before and after the experiment by gravimetric analysis, X-ray diffraction (XRD) and cross section electron microscopy analysis coupled with energy dispersive X-ray spectroscopy (EDS). All steels exposed for 30 days formed scales consisting mainly of metal (Cr, Fe, Ni) oxides showing different chemistry, microstructure and crystalline phases. Elemental iodine was only detected by EDS analysis in the scales of stainless steels 304 and 316. After 30 days, the Ti-Al exhibited no detectable scale, suggesting only a very thin film was formed. A scale consisting mainly of aluminum, iodine, and oxygen formed on the Al-Mg sample exposed to 30 days. Some pockets rich in magnesium, iodine and oxygen also formed in this Al-Mg alloy. Stainless steel 316, low carbon steel A36 and Ti-Al alloy coated with Silcolloy and stainless steel 304 coated with Dursan that were exposed for 30 days exhibited no oxidation. Stainless steel 304 coated with Silcolloy exposed for 30 days did not exhibit corrosion although the sample gained weight and the coating exhibited expansion. The weight gain per area performance of the materials exposed in iodine lamina flow containing oxygen at impurity level for 10, 15 and 30 days are reported from the lowest to the highest weight gain per area as follows: Steels: Less than 316 less than 304 less than A36; Ti-Al-Mg based alloys: Al-Mg less than Ti-Al: Considering the experimental uncertainties, no weight change was observed for Stainless steel 316, low carbon steel A36 and Ti-Al alloy coated with Silcolloy and stainless steel 304 coated with Dursan. The corrosion of the alloys is catalyzed by iodine in the presence of oxygen as impurity.

Costa, Gustavo C. C.↗

NASA Li/CF(x) cell problem analysis: Scanning electron microscopy with energy dispersive x ray spectrometry

An analysis was made of Lithium/carbon fluoride cell parts for possible chloride contamination induced by exposure to thionyl chloride (SOCl2); various samples were submitted for analysis. Only a portion of the analysis which has been conducted is covered, herein, namely analysis by scanning electron microscopy with energy dispersive x ray spectrometry (SEM/EDS). A strip of nickel was exposed to SOCl2 vapors to observe variations in surface concentrations of sulfur and chlorine with time. By detecting chlorine one can not infer contamination by SOCl2 only that contamination is present. Six samples of stainless steel foil were analyzed for chlorine using EDS. Chlorine was not detected on background samples but was detected on the samples which had been handled including those which had been cleaned. Cell covers suspected of being contaminated while in storage and covers which were not exposed to the same storage conditions were analyzed for chlorine. Although no chlorine was found on the covers from cells, it was found on all stored covers. Results are presented with techniques shown for analysis and identification. Relevant photomicrographs are presented.

Baker, John↗

Natural Fiber Simulations and Analysis for Composites

As the U.S. government and the aviation industry strive to achieve net-zero carbon emissions by 2050, the Sustainable Manufacturing of Aircraft (SUMAC) project, supported by the Convergent Aeronautics Solutions (CAS) program of the National Aeronautics and Space Administration (NASA), aims to develop sustainably derived thermoplastic composites and manufacturing technologies for future aviation. A multidisciplinary team of experts drives this initiative through a collective effort. The team’s key focus areas are sustainably derived thermoplastic resins, natural fiber reinforcement, composite manufacturing, structural health monitoring, computational materials modeling, and systems analysis. This presentation will give an overview of the SUMAC project. Fiber-scale microscopy analysis characterized fiber cross sections finding that hemp and flax fibers are very deformable and non-circular (circularities of 0.2 were observed), and diameters range from submicron to 20 μm. Fiber shapes range from flattened, with aspect ratios Rlong/Rshort up to 5, to round, Rlong/Rshort =1. And Fiber core perimeters, which likely drives deformability, were calculated Pcore=7 μm. Explicit-fiber yarn simulations, parameterized from single-fiber measurements, resolved and identified slack as a cause for yarn strain-hardening tensile behavior. The bonded network model of PLA, PHA and PA11 resins captures tensile behavior, and can model an infused weave. Computational models of the weave unit cells matched the pattern (including plain, twill and triaxial braid), yarn ply (1to 2), and yarn twist from optical microscopy.

thermoplastic↗

Natural Fiber Simulations and Analysis for Composites

As the U.S. government and the aviation industry strive to achieve net-zero carbon emissions by 2050, the Sustainable Manufacturing of Aircraft (SUMAC) project, supported by the Convergent Aeronautics Solutions (CAS) program of the National Aeronautics and Space Administration (NASA), aims to develop sustainably derived thermoplastic composites and manufacturing technologies for future aviation. A multidisciplinary team of experts drives this initiative through a collective effort. The team’s key focus areas are sustainably derived thermoplastic resins, natural fiber reinforcement, composite manufacturing, structural health monitoring, computational materials modeling, and systems analysis. This presentation will give an overview of the SUMAC project. Fiber-scale microscopy analysis characterized fiber cross sections finding that hemp and flax fibers are very deformable and non-circular (circularities of 0.2 were observed), and diameters range from submicron to 20 μm. Fiber shapes range from flattened, with aspect ratios Rlong/Rshort up to 5, to round, Rlong/Rshort =1. And Fiber core perimeters, which likely drives deformability, were calculated Pcore=7 μm. Explicit-fiber yarn simulations, parameterized from single-fiber measurements, resolved and identified slack as a cause for yarn strain-hardening tensile behavior. The bonded network model of PLA, PHA and PA11 resins captures tensile behavior, and can model an infused weave. Computational models of the weave unit cells matched the pattern (including plain, twill and triaxial braid), yarn ply (1to 2), and yarn twist from optical microscopy.

thermoplastic↗

New Method Developed To Purify Single Wall Carbon Nanotubes for Aerospace Applications

Single wall carbon nanotubes have attracted considerable attention because of their remarkable mechanical properties and electrical and thermal conductivities. Use of these materials as primary or secondary reinforcements in polymers or ceramics could lead to new materials with significantly enhanced mechanical strength and electrical and thermal conductivity. Use of carbon-nanotube-reinforced materials in aerospace components will enable substantial reductions in component weight and improvements in durability and safety. Potential applications for single wall carbon nanotubes include lightweight components for vehicle structures and propulsion systems, fuel cell components (bipolar plates and electrodes) and battery electrodes, and ultra-lightweight materials for use in solar sails. A major barrier to the successful use of carbon nanotubes in these components is the need for methods to economically produce pure carbon nanotubes in large enough quantities to not only evaluate their suitability for certain applications but also produce actual components. Most carbon nanotube synthesis methods, including the HiPCO (high pressure carbon monoxide) method developed by Smalley and others, employ metal catalysts that remain trapped in the final product. These catalyst impurities can affect nanotube properties and accelerate their decomposition. The development of techniques to remove most, if not all, of these impurities is essential to their successful use in practical applications. A new method has been developed at the NASA Glenn Research Center to purify gram-scale quantities of single wall carbon nanotubes. This method, a modification of a gas phase purification technique previously reported by Smalley and others, uses a combination of high-temperature oxidations and repeated extractions with nitric and hydrochloric acid. This improved procedure significantly reduces the amount of impurities (catalyst and nonnanotube forms of carbon) within the nanotubes, increasing their stability significantly. The onset of decomposition of the purified nanotubes (determined by thermal gravimetric analysis in air) is more than 300 C higher than that of the crude nanotubes. Transmission electron microscopy analysis of nanotubes purified by this method reveals near complete removal of iron catalyst particles. Analysis of the nanotubes using inductively coupled plasma spectroscopy revealed that the iron content of the nanotubes was reduced from 22.7 wt% in the crude nanotubes to less than 0.02 wt%. X-ray photoelectron spectroscopy revealed a decrease in iron content after purification as well as an increase in oxygen content due to the formation of carboxylic acid groups on the surface of the nanotubes. Nanotubes purified by this improved method can be readily dispersed in common organic solvents, in particular N,N-dimethylformamide, using prolonged ultrasonic treatment. These dispersions can then be used to incorporate single wall carbon nanotubes into polymer films.

Lebron, Marisabel↗

Chemical and Microstructural Changes in Metallic and Ceramic Materials Exposed to Venusian Surface Conditions

The chemical and microstructural behavior of steels (304, 310, 316, and 1018), nickel-based alloys (beta-NiAl, G30, and 625), gold, coatings (4YSZ, SilcoNert(TradeMark) 1040 (SilcoTek Co.), Dursan(TradeMark) (SilcoTek Co.), and porcelain), and bulk ceramics (alpha-Al2O3, fused quartz, beta-SiC, and alpha-Si3N4) were probed after exposure to supercritical fluid with temperature, pressure, and composition mimicking the Venus lower atmosphere. Exposures were carried out in the Glenn Extreme Environments Rig (GEER) chamber with the Venusian gas mixture (96.5% CO2, 3.5% N2, 30 ppm H2O, 150 ppm SO2, 28 ppm CO, 15 ppm OCS, 3 ppm H2S, 0.5 ppm HCl, and 5 ppb HF) at 92 bar (1330 psi) and 467 C (873 F) for durations of 10 and 42 days. An additional 21-day exposure was done to stainless steel uncoated and coated with SilcoNert(TradeMark) and Dursan(TradeMark). Samples were characterized before and after the experiment by gravimetric analysis, X-ray diffraction, X-ray photoelectron and Auger electron spectroscopies, and cross section electron microscopy analysis. All steels exposed for 10 and 42 days formed double-layered scales consisting mainly of metal (Cr, Fe, Ni) oxides and sulfides showing different chemistry, microstructure, and crystalline phases. The alloys G30 and 625 formed double-layered scales consisting mainly of nickel sulfides. After 10 days, the beta-NiAl exhibited no detectable scale, suggesting only a very thin film was formed. The 304 and 316 stainless steels coated with 4YSZ that were exposed for 10 and 42 days exhibited no significant oxidation. Steel 1018 coated with 4YSZ exhibited a corrosion scale of iron and/or chromium oxide formed at the base of the alloy. The 304 steel coated with porcelain did not exhibit corrosion, although the coating exhibited recession. SilcoNert(TradeMark) exposed for 10 and 42 days exhibited recession, although no oxidation was found to occur at the base of the alloy. Stainless steel 316 coated with Dursan(TradeMark)  exhibited corrosion at the base of the alloy. All ceramics tested showed no clear evidence of reaction. The weight-gain-per-area performance of the materials exposed in the GEER for 10 and 42 days are reported from the lowest to the highest weight gain per area as follows: gold did not exhibit any weight change; nickel-based alloys: beta- NiAl < G30 < 625; steels: 304 < 310 < 316 < 1018; ceramics: considering the experimental uncertainties, no weight change was observed for all ceramics of this work (alpha-Al2O3, Si3N4, SiC, and amorphous SiO2).

Costa, Gustavo C. C.↗

Control of wetting and uniformity via ZrSi x formation in ceramic-to-metal joints fabricated using Ag-Zr brazes

The deposition of a 2.0 µm SiO 2 film on the alumina surface in Kovar TM /94% alumina joints enables the formation of a silicide reaction layer on the alumina during brazing with 97Ag2Zr1Cu. Additionally, the average and standard deviation of joint thickness decrease from 50 to 15 and 29 to 4 µm, respectively compared to joints without added SiO 2 . Finally, the average failure stress of these braze joints was 45 MPa, while that of similar joints without added SiO 2 was 90 MPa. Sessile drop experiments of 98Ag2Zr on SiO 2 and 99.6% Al 2 O 3 substrates show that the braze wets and spreads to 3x its original area on SiO 2 with a wetting angle near 0°, but remains the same area on 99.6% Al 2 O 3 with a wetting angle of 106.6°. Focused-ion-beam scanning electron microscopy analysis of a cross-section of the 98Ag2Zr sessile drop on the SiO 2 substrate has shown that Zr reacts with SiO 2 to form Zr oxide and silicide layers. Scanning transmission electron microscopy diffraction and energy dispersive X-ray spectroscopy analysis indicate this silicide layer contains tetragonal Zr 5 Si 4 . In conclusion, analysis shows the silicide layer enhances wetting and joint uniformity while unreacted SiO 2 embrittles the joint and degrades strength.

alumina↗