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Transmission electron microscopy and optical microscopy were used to examine polycrystalline specimens of the B2-structured alloy FeAl strained under tension to fracture at elevated temperature. Strain-induced grain boundary migration was observed above 900 K and dynamic recrystallization was found at 1000 K and 1100 K. Little evidence of dynamic recovery was evident but some networks were formed at 1100 K.
Bilgewater emulsions, consisting of oil and surfactant mixtures in water, affect many aquatic species. Thus development of methods and techniques to treat or mitigate the formation and undesired consequences of shipboard emulsions are urgently needed. This work presents new results of the evolution of the bilgewaer chemical and physical properties using in situ imaging. A Navy O/W emulsion consisting of three oils and a detergent mixture was used as the synthetic bilgewater model [1, 2]. Synthetic oil-in-water (O/W) emulsion droplets were seled in a vacuum compatible microfluidic sample holder and imaged using a suite of tools including scanning electron microscopy (SEM), time-of-flight secondary ion mass spectrometry (ToF-SIMS), confocal laser scanning microscopy, and optical microscopy, highlighting the advantage of multiscale analysis and its applications in waste reduction and treatment in the environment. The transferrable and vacuum compatible microfluidic interface, System for Analysis at the Liquid Vacuum Interface (SALVI), was used in this study. SALVI enabled surface analysis of liquids and liquid-solid interactions using ToF-SIMS and SEM [3, 4]. Its detection window is an aperture of 2 ?m in diameter open to vacuum, permitting direct detection of the liquid surface. Liquid is withheld by surface tension within the aperture. The interface is composed of a silicon nitride membrane and polydimethylsiloxane microchannel [3, 4]. A variety of samples including complex liquid mixtures, ionic liquids, single mammalian cells, live biofilms, and solid-electrolyte interface have been analyzed using in situ imaging [5, 6]. The feasibility of using SALVI for in situ SEM imaging of nanoparticles and colloids in liquid was recently demonstrated [7]. This paper shows new findings of multimodal imaging and analysis of synthesized emulsion particles in water. Figure 1 depicts a schematic of multimodal in situ imaging of bilgewater emulsion using SEM and ToF-SIMS. Furthermore, we study the interactions of microbes and bilgewater emulsion. Microbes play an important role in the ocean. We hypothesize that microbes release organics that can act as surfactants that affect bilgewater formation or weakening. We present the first systematic study of emulsions and biofilms and investigate the effects of biofilms on bilgewater emulsions. Pseudomonas was selected as a model strain. Biofilms were cultured in a microchannel to allow culture [8]. Once a thick layer of biofilms was formed, the medium solution was changed to a mixture consisting of 50 % bilgewater emulsion. Dispersed biofilms were collected at 24 hrs. and 48 hrs. after emulsions were introduced into the channel. Bilgewater emulsions, biofilms, and mixtures of bilgewater emulsions and biofilms were analyzed using multiple in situ and ex situ techniques as described earlier. Our findings indicate that biofilms change the chemical makeup of the emulsion surface compositions and emulsion droplet size distribution, confirming the hypothesis that extracellular polymeric substance (EPS) related components released from biofilms can function as surfactants and change the oil-in-water interfaces.
Refractive indices of new nonlinear optical materials based on 4-nitrophenol cocrystals with the aminopyridines 2-aminopyridine, 2,6-aminopyridine, and 4-aminopyridine have been studied. The refractive indices of the compounds under study are presented: n = 1.694 (optical microscopy) and 1.605 (Abbe method) for 2-aminopyridine-4-nitrophenol (2AP4N), n = 1.541 (optical microscopy) and 1.589 (Abbe method) for 2,6-diaminopyridine-4-nitrophenol (2,6DAP4N), and n = 1.561 (optical microscopy) and 1.591 (Abbe method) for 4-aminopyridine-4-nitrophenol (4AP4N).
An effect of the friction stir processing (FSP), its pass numbers and addition of the SiO{sub 2} nanoparticles on microhardness, wear behavior and corrosion performance of the Al6061 aluminum alloy was investigated. Scanning electron microscopy (SEM) and optical microscopy were utilized to characterize the microstructure of the alloy, FSPed and composite samples. SEM observations revealed that the SiO{sub 2} particles were not uniformly dispersed in the matrix after two passes of FSP. However, increasing the pass number more than two passes resulted in a great improvement in the distribution of the SiO{sub 2} particles. The application of FSP led to overall softening compared to the base metal. Softening of the Al6061 alloy was probably attributed to the coarsening of Mg{sub 2}Si. Corrosion resistance of the FSPed samples found a significant reduction compared to the base metal. Applying higher pass number of the process and also addition of the SiO{sub 2} nanoparticles improved the wear behavior of the samples.
Enhancing the reliability and reproducibility of optical microscopy by reducing specimen irradiance continues to be an important biotechnology target. As irradiance levels are reduced, however, the particle nature of light is heightened, giving rise to Poisson noise, or photon sparsity that restricts only a few (0.5%) image pixels to comprise a photon. Photon sparsity can be addressed by collecting approximately 200 photons per pixel; this, however, requires long acquisitions and, as such, suboptimal imaging rates. Here, we introduce near-zero photon bioimaging, a method that operates at kHz rates and 10,000-fold lower irradiance than standard microscopy. To achieve this level of performance, we uniquely combined a judiciously designed epifluorescence microscope enabling ultralow background levels and AI that learns to reconstruct biological images from as low as 0.01 photons per pixel. We demonstrate that near-zero photon bioimaging captures the structure of multicellular and subcellular features with high fidelity, including features represented by nearly zero photons. Beyond optical microscopy, the near-zero photon bioimaging paradigm can be applied in remote sensing, covert applications, and biomedical imaging that utilize damaging or quantum light.
The ability to determine the in situ optoelectronic properties of semiconductor materials has become especially important as the size of device architectures has decreased and the development of complex microsystems has increased. Scanning Tunneling Optical Resonance Microscopy, or STORM, can interrogate the optical bandgap as a function of its position within a semiconductor micro-structure. This technique uses a tunable solidstate titanium-sapphire laser whose output is "chopped" using a spatial light modulator and is coupled by a fiber-optic connector to a scanning tunneling microscope in order to illuminate the tip-sample junction. The photoenhanced portion of the tunneling current is spectroscopically measured using a lock-in technique. The capabilities of this technique were verified using semiconductor microstructure calibration standards that were grown by organometallic vapor-phase epitaxy. Bandgaps characterized by STORM measurements were found to be in good agreement with the bulk values determined by transmission spectroscopy and photoluminescence and with the theoretical values that were based on x-ray diffraction results.
This presentation is about the leveraging super high optical resolution microscopy to probe the interaction zone between clostritium thermocellum and biomass.
During the ten-week internship, my work focused on synthesis, characterization, and tailoring the flowability of the MAB phase powders for improving the surface finish and decreasing porosity of 3D-printed MAB phase structures. My mentor for the project was Dr. Samuel Hocker from NASA Langley and my faculty advisor was Dr. Surojit Gupta from the University of North Dakota. I also collaborated with Daniel Trieff from the University of North Dakota in developing characterization paradigm of 3D printed samples. The microencapsulation was performed via novel solvent casting-based microencapsulation process pioneered in UND, wherein a polymer (PLA, PHA) was dissolved into dichloromethane and precipitated onto the surface of the MoAlB particles. Two 100mL samples of microencapsulated powder was outsourced to Particle Technology Labs for flowability testing along with a 100mL control sample to determine if microencapsulation is a valid method for improving the flowability. The microencapsulated powders were characterized using SEM, Differential Scanning Calorimetry, and optical microscopy. The SEM images showed no change between the pure and microencapsulated powders. The optical microscopy analysis indicated a reduction in reflectivity for the PLA microencapsulated powders as well as hydrophobic properties. Both results suggest that microencapsulation was successful as PLA is a hydrophobic polymer and the change in reflectivity could be a result of the light being dispersed through the polymer coating. A reflectivity analysis will be done to bring more perspective to these observations. If powder flowability is improved, then the project will move forward with testing the printability of the microencapsulated powders and characterizing the structures using the designed characterization protocol. We are waiting for the DSC results. The characterization protocol for the 3D-printed MAB structures included a visual inspection of the plates to rule out any samples that had spalled or delaminated, optical microscopy to document surface features, porosity, and decomposition, and cleaning of the plates using an ultrasonic bath in preparation for SEM, EDS, and profilometry analyses.
This poster, part of the Pacific Northwest National Laboratory-sponsored Integration 2020: Visualizing the Proteome virtual conference, discusses super high optical resolution microscopy to probe the interaction zone between Clostritium thermocellum and biomass. Clostridium thermocellum is one of the most efficient microorganisms for the deconstruction of biomass. To achieve this high level of cellulolytic activity, C. thermocellum uses large multienzyme complexes known as cellulosomes to sugars in 4-5 break down polysaccharides found in plant cell walls. The attachment of bacterial switchgrass 70% cells to the nearby substrate via the cellulosome has been hypothesized to be the reason for this high efficiency. The region lying between the cell and the substrate has shown great variation and dynamics that are affected by the growth stage of cells and the substrate used for growth.
Using higher-resolution wide-field computational optical-sectioning fluorescence microscopy, the distribution of antigens recognized by antibodies against animal beta 1 integrin, fibronectin, and vitronectin has been visualized at the outer surface of enzymatically protoplasted onion epidermis cells and in depectinated cell wall fragments. On the protoplast all three antigens are colocalized in an array of small spots, as seen in raw images, in Gaussian filtered images, and in images restored by two different algorithms. Fibronectin and vitronectin but not beta 1 integrin antigenicities colocalize as puncta in comparably prepared and processed images of the wall fragments. Several control visualizations suggest considerable specifity of antibody recognition. Affinity purification of onion cell extract with the same anti-integrin used for visualization has yielded protein that separates in SDS-PAGE into two bands of about 105-110 and 115-125 kDa. These bands are again recognized by the visualization antibody, which was raised against the extracellular domain of chicken beta 1 integrin, and are also recognized by an antibody against the intracellular domain of chicken beta 1 integrin. Because beta 1 integrin is a key protein in numerous animal adhesion sites, it appears that the punctate distribution of this protein in the cell membranes of onion epidermis represents the adhesion sites long known to occur in cells of this tissue. Because vitronectin and fibronection are matrix proteins that bind to integrin in animals, the punctate occurrence of antigenically similar proteins both in the wall (matrix) and on enzymatically prepared protoplasts reinforces the concept that onion cells have adhesion sites with some similarity to certain kinds of adhesion sites in animals.
Environments that impose operational constraints on conventional silicon-(Si) based semiconductor devices frequently appear in military- and space-grade applications. These constraints include high temperature, high power, and high radiation environments. Silicon carbide (SiC), an alternative type of semiconductor material, has received abundant research attention in the past few years, owing to its radiation-hardened properties as well as its capability to withstand high temperatures and power levels. However, the growth and manufacture of SiC devices is still comparatively immature, and there are severe limitations in present crystal growth and device fabrication processes. Among these limitations is a variety of crystal imperfections known as defects. These imperfections can be point defects (e.g., vacancies and interstitials), line defects (e.g., edge and screw dislocations), or planar defects (e.g., stacking faults and double-positioning boundaries). All of these defects have been experimentally shown to be detrimental to the performance of electron devices made from SiC. As such, it is imperative that these defects are significantly reduced in order for SiC devices to become a viable entity in the electronics world. The NASA Glenn High Temperature Integrated Electronics & Sensors Team (HTIES) is working to identify and eliminate these defects in SiC by implementing improved epitaxial crystal growth procedures. HTIES takes two-inch SiC wafers and etches patterns, producing thousands of mesas into each wafer. Crystal growth is then carried out on top of these mesas in an effort to produce films of improved quality-resulting in electron devices that demonstrate superior performance-as well as fabrication processes that are cost-effective, reliable, and reproducible. In this work, further steps are taken to automate HTIES' SiC wafer inspection system. National Instruments LabVIEW image processing and pattern recognition routines are developed that are capable of quantifying and mapping defects on both the substrate and mesa surfaces, and of quantifying polymorphic changes in the grown materials. In addition, an optical emission microscopy (OEM) system is developed that will facilitate comprehensive study of recombination-enhanced dislocation motion (REDM).
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.
Polymer matrix composites (PMCs) are increasingly used in aerospace and automotive applications because of their light weight and high strength-to-weight ratio relative to metals. However, a major drawback of PMCs is poor abrasion resistance, which restricts their use, especially at high temperatures. Simply applying a hard coating on PMCs to improve abrasion and erosion resistance is not effective since coating durability is short lived (ref. 1). Generally, PMCs have higher coefficients of thermal expansion than metallic or ceramic coatings have, and coating adhesion suffers because of poor interfacial adhesion strength. One technique commonly used to improve coating adhesion or durability is the use of bond coats that are interleaved between a coating and a substrate with vastly different coefficients of thermal expansion. An example of this remedy is the use of bondcoats for ceramic thermal barrier coatings on metallic turbine components (ref. 2). Prior collaborative research between the NASA Glenn Research Center and the Allison Advanced Development Company (AADC) demonstrated that bond coats sandwiched between PMCs and high-quality plasma-sprayed, erosion-resistant coatings substantially improved the erosion resistance of PMCs (ref. 3). One unresolved problem in this earlier collaboration was that there was no easy, accurate way to measure the coating erosion wear scar. Coating wear was determined by both profilometry and optical microscopy. Both techniques are time consuming. Wear measurement by optical microscopy requires sample destruction and does not provide a comprehensive measure of the entire wear volume. An even more subtle, yet critical, problem is that these erosion coatings contain two or more materials with different densities. Therefore, simply measuring specimen mass loss before and after erosion will not provide an accurate gauge for coating and/or substrate volume loss. By using a noncontact technique called scanning optical interferometry, which was recently developed at Glenn, researchers can accurately determine the wear performance of erosion-coated PMCs while preserving the sample. An example of this interferometry technique is shown in the preceding figure for an erosion-coated inlet guide vane from a Rolls Royce AE3007 regional gas turbine jet engine. Erosion was conducted with coated and uncoated PMC vanes, with the abrasive material moving at a velocity of 229 m/s at impingement angles of 20 and 90 degrees. The coatings for PMCs remarkably reduced the erosion volume loss by a factor of approximately 10. Currently, several erosion coatings for PMCs are being compared and downselected for engine testing at Rolls Royce.
We study the protein-directed assembly of colloidal gold nanoparticles on de novo designed protein nanofiber templates. Using sequential assembly on glass substrates, we attach of positively-charged gold nanoparticles to protein nanofibers engineered to have a high density of negatively-charged surface residues. Using a combination of electron and optical microscopy, we measure the density of particle attachment and characterize binding specificity. By varying nanoparticle size and pH of the solution, we explore the importance of charge-dependent particle-fiber and particle-substrate interactions. We find an inverse correlation between particle size and attachment density to the protein nanofibers, attributed to the balance between size-dependent electrostatic particle-fiber attraction and particle-substrate repulsion. We show pH-dependent particle attachment density and binding specificity in relation to the protonation fraction of each assembly layer. Finally, we employ hyperspectral scattering microscopy to draw conclusions about particle density and interparticle spacings of optically-observable particle assemblies.
α-RuCl 3 , a narrow-band Mott insulator with a large work function, offers intriguing potential as a quantum material or as a charge acceptor for electrical contacts in van der Waals devices. In this work, we perform a systematic study of the optical reflection contrast of α-RuCl 3 nanoflakes on oxidized silicon wafers and estimate the accuracy of this imaging technique to assess the crystal thickness. Via spectroscopic micro-ellipsometry measurements, we characterize the wavelength-dependent complex refractive index of α-RuCl 3 nanoflakes of varying thickness in the visible and near-infrared. Building on these results, we simulate the optical contrast of α-RuCl 3 nanoflakes with thicknesses below 100 nm on SiO 2 /Si substrates under different illumination conditions. We compare the simulated optical contrast with experimental values extracted from optical microscopy images and obtain good agreement. Finally, we show that optical contrast imaging allows us to retrieve the thickness of the RuCl 3 nanoflakes exfoliated on an oxidized silicon substrate with a mean deviation of –0.2 nm for thicknesses below 100 nm with a standard deviation of only 1 nm. Our results demonstrate that optical contrast can be used as a non-invasive, fast, and reliable technique to estimate the α-RuCl 3 thickness.
During the Hubble Space Telescope (HST) Second Servicing Mission, 6.8 years after the telescope was deployed in low Earth orbit, degradation of unsupported Teflon FEP (DuPont; fluorinated ethylene propylene), used as the outer layer of the multilayer insulation (MLI) blankets, was evident as large cracks on the telescope light shield. A sample of the degraded outer layer (see the photograph) was retrieved during the second servicing mission and returned to Earth for ground testing and evaluation. Also retrieved was a Teflon FEP radiator surface from a cryogen vent cover that was exposed to the space environment on the aft bulkhead of the HST. NASA Goddard Space Flight Center directed the efforts of the Hubble Space Telescope MLI Failure Review Board, whose goals included determining the FEP degradation mechanisms. As part of the investigations into the degradation mechanisms, specimens retrieved from the first and second HST servicing missions, 3.6 and 6.8 years after launch, respectively, were characterized through exhaustive mechanical, optical, and chemical testing. Testing led by Goddard included scanning electron microscopy, optical microscopy, tensile testing, solar absorptance measurements, time-of-flight secondary ion mass spectroscopy (TOF-SIMS), Fourier transform infrared microscopy (m-FTIR), attenuated total reflectance infrared microscopy (ATR/FTIR), and x-ray diffraction (XRD). The NASA Lewis Research Center contributed significantly to the analysis of the retrieved HST materials by leading efforts and providing results of bend testing, surface microhardness measurements, x-ray photoelectron spectroscopy, solid-state nuclear magnetic resonance spectroscopy, and density measurements. Other testing was conducted by Nano Instruments, Inc., and the University of Akron.
Fiber optic window fitted to stainless steel field ion microscope permitting use of direct contact photography for image recording
This report demonstrates tunable carrier densities in CdO thin films through local ion irradiation, providing lateral control of mid‐IR optical properties. Ion‐solid interactions produce donor‐like defects that boost electron concentrations from the practical minimum of 2.5 × 10 19 cm −3 to a maximum of 2.5 × 10 20 cm −3 by metered ion exposure. This range is achieved using He, N, Ar, or Au ions at 1–2.8 MeV; when normalized by displacements per atom, all ion species produce comparable results. Since CdO is well‐described by the Drude model, irradiation‐tuned carrier densities directly alter the infrared dielectric function, and in turn, mid‐infrared optical properties. Further, it is demonstrated that by combining irradiation with traditional lithography, CdO films expose to ions in the presence of 3‐µm thick, patterned photoresist exhibit lateral carrier density profiles with ≈400‐nm resolution. Scanning near‐field optical microscopy reveals sharp optical interfaces with almost no companion contrast in surface morphology, microstructure, or crystallinity. Finally, CdO lateral homostructures supporting surface plasmon polaritons (SPPs) are demonstrated whose dispersion relation can be tuned through periodic patterning in a monolithic platform by simple nanofabrication. Numerical simulations show these polaritons result from strong coupling between excitations at CdO plasma frequencies and SPPs supported by the platinum substrate.