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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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Electron microscope, electron diffraction, and electron microprobe analysis of defective solid state weldment on liquid hydrogen tank from Apollo 12 fuel cell system
Abstract not provided.
Electron microscopes (EM’s), are workhorse tools serving diverse fields such as materials science, biological science, and engineering. Scanning EM’s (SEM’s) in particular enable high magnification study and pinpoint chemical analyses of structures down to the nanoscale by providing a powerful blend of strong optical scattering, high native resolution, large depth of focus, and energy-dispersive X-ray spectroscopy (EDS). Mochii is the world’s smallest production electron microscope, scheduled to travel to the International Space Station (ISS) this spring where it will serve as an ISS National Laboratory (ISSNL) microgravity facility on successful demonstration. We previously reported on progress preparing Mochii for space flight, in particular flight integration verifications and science application testing. These included standard integration testing such as electromagnetic interference and flight vibration, and extend to unique functional testing such as magnetic susceptibility and extreme analog environment testing under the sea. Presently, Mochii payload flight hardware has completed testing and was handed over to NASA’s ISS payload processing facility in Houston. It will make its way to the the east coast for launch currently scheduled on Space-X CRS-20 for Mission increment 62 in March 2020.
Electron microscope producing dark field images without resolution loss, using primary beam electrical tilting
Two screws and two washers, several small chips of tubing, and a fiber removed from a third screw were examined with the scanning electron microscope and the electron microprobe. The purpose of the examination was to determine the nature of the material on the surface of these samples and to search for the presence of meteoritic material.
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A new experimental framework for the characterization of defects in semiconductors is demonstrated. Through the direct, energy-resolved correlation of three analytical techniques spanning six orders of magnitude in spatial resolution, a critical mid-bandgap electronic trap level (E V + 0.56 eV) within Ag 0.2 Cu 0.8 In 1–x Ga x Se 2 is traced to its nanoscale physical location and chemical source. This is achieved through a stepwise, site-specific correlated characterization workflow consisting of device-scale (≈1 mm 2 ) deep level transient spectroscopy (DLTS) to survey the traps present, scanning probe–based DLTS (scanning-DLTS) for mesoscale-resolved (hundreds of nanometers) mapping of the target trap state’s spatial distribution, and scanning transmission electron microscope based electron energy-loss spectroscopy (STEM-EELS) and X-ray energy-dispersive spectroscopy for nanoscale energy-, structure, and chemical-resolved investigation of the defect source. Furthermore, this first demonstration of the direct observation of sub-bandgap defect levels via STEM-EELS, combined with the DLTS methods, provides strong evidence that the longsuspected Cu In/Ga substitutional defects are indeed the most likely source of the E V + 0.56 eV trap state and serves as a key example of this approach for the fundamental identification of defects within semiconductors, in general.
Scanning electron microscope for evaluating failure mechanisms in semiconductor devices, and for three-dimensional representation of biological specimens
An electron microscope is described with an electron source a condenser lens having either a circular aperture for focusing a solid cone of electrons onto a specimen or an annular aperture for focusing a hollow cone of electrons onto the specimen. It also has objective lens with an annular objective aperture, for focusing electrons passing through the specimen onto an image plane. A method of making the annular objective aperture using electron imaging, electrolytic deposition and ion etching techniques is included.
Electron microscopy and defect analysis are a cornerstone of materials science, as they offer detailed insights on the microstructure and performance of a wide range of materials and material systems. Building a robust and flexible platform for automated defect recognition and classification in electron microscopy will result in the completion of analysis orders of magnitude faster after images are recorded, or even online during image acquisition. Automated analysis has the potential to be significantly more efficient, accurate, and repeatable than human analysis, and it can scale with the increasingly important methods of automated data generation. Herein, an automated recognition tool is developed based on a computer vison–based approach; it sequentially applies a cascade object detector, convolutional neural network, and local image analysis methods. We demonstrate that the automated tool performs as well as or better than manual human detection in terms of recall and precision and achieves quantitative image/defect analysis metrics close to the human average. The proposed approach works for images of varying contrast, brightness, and magnification. Furthermore, these promising results suggest that this and similar approaches are worth exploring for detecting multiple defect types and have the potential to locate, classify, and measure quantitative features for a range of defect types, materials, and electron microscopic techniques.
Scanning electron microscopes are used to determine both user-induced damages and manufacturing defects subtle enough to be missed by conventional light microscopy. Method offers greater depth of field and increased working distances.
Here, this article describes the establishment, over a period of 10 years or so, of a multi-user, institution-wide facility for the characterization of materials and devices at the nanoscale. Emphasis is placed on the type of equipment that we have found to be most useful for our users, and the business strategy that maintains its operations. A central component of our facility is an aberration-corrected environmental transmission electron microscope and its application is summarized in the studies of plasmon energies of silver nanoparticles, the band gap of PbS quantum dots, atomic site occupancy near grain boundaries in yttria stabilized zirconia, the lithiation of silicon nanoparticles, in situ observations on carbon nanotube oxidation and the electron tomography of varicella zoster virus nucleocapsids.
The scanning electron microscope is becoming a popular tool to perform tasks that require positioning, manipulation, characterization, and assembly of micro-components. However, some of these applications require a higher level of performance with respect to dynamics and precision of positioning. One limiting factor is the presence of unidentified noises and disturbances. This work aims to study the influence of mechanical disturbances generated by the environment and by the microscope, identifying how these can affect elements in the vacuum chamber. To achieve this objective, a dedicated setup, including a high-resolution vibrometer, was built inside the microscope. This work led to the identification and quantification of main disturbances and noise sources acting on a scanning electron microscope. Furthermore, the effects of external acoustic excitations were analysed. Potential applications of these results include noise compensation and real-time control for high accuracy tasks.
In-situ (scanning) transmission electron microscopy (S/TEM) is being developed for numerous applications in the study of nucleation and growth under electrochemical driving forces. For this type of experiment, one of the key parameters is to identify when nucleation initiates. Typically the process of identifying the moment that crystals begin to form is a manual process requiring the user to perform an observation and respond accordingly (adjust focus, magnification, translate the stage etc.). However, as the speed of the cameras being used to perform these observations increases, the ability of a user to “catch” the important initial stage of nucleation decreases (there is more information that is available in the first few milliseconds of the process). Here we show that video shot boundary detection (SBD) can automatically detect frames where a change in the image occurs. We show that this method can be applied to quickly and accurately identify points of change during crystal growth. This technique allows for automated segmentation of a digital stream for further analysis and the assignment of arbitrary time stamps for the initiation of processes that are independent of the user’s ability to observe and react.
Presented here is a protocol for preparing cryo-lamellae from plunge-frozen grids of Plasmodium falciparum-infected human erythrocytes, which could easily be adapted for other biological samples. The basic principles for preparing samples, milling, and viewing lamellae are common to all instruments and the protocol can be followed as a general guide to on-grid cryo-lamella preparation for cryo-electron microscopy (cryoEM) and cryo-electron tomography (cryoET). Electron microscopy grids supporting the cells are plunge-frozen into liquid nitrogen-cooled liquid ethane using a manual or automated plunge freezer, then screened on a light microscope equipped with a cryo-stage. Frozen grids are transferred into a cryo-scanning electron microscope equipped with a focused ion beam (cryoFIB-SEM). Grids are routinely sputter coated prior to milling, which aids dispersal of charge build-up during milling. Alternatively, an e-beam rotary coater can be used to apply a layer of carbon-platinum to the grids, the exact thickness of which can be more precisely controlled. Once inside the cryoFIB-SEM an additional coating of an organoplatinum compound is applied to the surface of the grid via a gas injection system (GIS). This layer protects the front edge of the lamella as it is milled, the integrity of which is critical for achieving uniformly thin lamellae. Regions of interest are identified via SEM and milling is carried out in a step-wise fashion, reducing the current of the ion beam as the lamella reaches electron transparency, in order to avoid excessive heat generation. A grid with multiple lamellae is then transferred to a transmission electron microscope (TEM) under cryogenic conditions for tilt-series acquisition. A robust and contamination-free workflow for lamella preparation is an essential step for downstream techniques, including cellular cryoEM, cryoET, and sub-tomogram averaging. Development of these techniques, especially for lift-out and milling of high-pressure frozen samples, is of high-priority in the field.
Abstract not provided