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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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At least 73 records · Page 4

Investigating Li Microstructure Formation on Li Anodes for Lithium Batteries by $In Situ$ 6 Li/ 7 Li NMR and SEM

The growth of lithium microstructures during battery cycling has, to date, prohibited the use of Li metal anodes and raises serious safety concerns even in conventional lithium-ion rechargeable batteries, particularly if they are charged at high rates. The electrochemical conditions under which these Li microstructures grow have, therefore, been investigated by in situ nuclear magnetic resonance (NMR), scanning electron microscopy (SEM), and susceptibility calculations. Lithium metal symmetric bag cells containing LiPF 6 in EC/DMC electrolytes were used. Distinct 7 Li NMR resonances were observed due to the Li metal bulk electrodes and microstructures, the changes in peak positions and intensities being monitored in situ during Li deposition. The changes in the NMR spectra, observed as a function of separator thickness and porosity (using Celgard and Whatmann glass microfiber membranes) and different applied pressures, were correlated with changes in the type of microstructure, by using SEM. Isotopically enriched 6 Li metal electrodes were used against natural abundance predominantly 7 Li metal counter electrodes to investigate radiofrequency (rf) field penetration into the Li anode and to confirm the assignment of the higher frequency peak to Li dendrites. The conclusions were supported by calculations performed to explore the effect of the different microstructures on peak position/broadening, the study showing that Li NMR spectroscopy can be used as a sensitive probe of both the amount and type of microstructure formation.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Adapting the Electron Beam from SEM as a Quantitative Heating Source for Nanoscale Thermal Metrology

The electron beam (e-beam) in the scanning electron microscopy (SEM) provides an appealing mobile heating source for thermal metrology with spatial resolution of ~1 nm, but the lack of systematic quantification of the e-beam heating power limits such application development. Here, we systemically study e-beam heating in LPCVD silicon nitride (SiN x ) thin-films with thickness ranging from 200 to 500 nm from both experiments and complementary Monte Carlo simulations using the CASINO software package. There is good agreement about the thickness-dependent e-beam energy absorption of thin-film between modeling predictions and experiments. Using the absorption results, we then demonstrate adapting the e-beam as a quantitative heating source by measuring the thickness-dependent thermal conductivity of SiN x thin-films, with the results validated to within 7% by a separate Joule heating experiment. The results described here will open a new avenue for using SEM e-beams as a mobile heating source for advanced nanoscale thermal metrology development.

42 ENGINEERING↗

Correlative SIP-FISH-Raman-SEM-NanoSIMS links identity, morphology, biochemistry, and physiology of environmental microbes

Microscopic and spectroscopic techniques are commonly applied to study microbial cells but are typically used on separate samples, resulting in population-level datasets that are integrated across different cells with little spatial resolution. To address this shortcoming, we developed a workflow that correlates several microscopic and spectroscopic techniques to generate an in depth analysis of individual cells. By combining stable isotope probing (SIP), fluorescence in situ hybridization (FISH), scanning electron microscopy (SEM), confocal Raman microspectroscopy (Raman), and nano-scale secondary ion mass spectrometry (NanoSIMS), we illustrate how individual cells can be thoroughly interrogated to obtain information about their taxonomic identity, structure, physiology, and metabolic activity. Analysis of an artificial community demonstrated that our correlative approach was able to resolve the activity of single cells using heavy water SIP in conjunction with Raman and/or NanoSIMS and establish their taxonomy and morphology using FISH and SEM. We then applied this workflow to a sample of yet uncultured multicellular magnetotactic bacteria. In addition to establishing their identity and activity, backscatter electron microscopy (BSE), NanoSIMS, and energy-dispersive X-ray spectroscopy (EDS) were employed to characterize the magnetosomes within the cells. By integrating these techniques, we demonstrate a cohesive approach to thoroughly study environmental microbes at single cell resolution.

Schaible, George↗

X-ray diffraction, FTIR, UV-VIS and SEM studies on chromium (III) complexes

Five Chromium (III) complexes have been prepared using Schiff base ligands which derived from benzoin and five different amino acids (H{sub 2}N-R). Samples were characterized by XRD, FTIR, UV-VIS and SEM method. X-Ray diffraction pattern analyzed that all chromium (III) complexes have hexagonal structure and crystalline, in nature, using Bruker D8 Advance instrument. Using VERTAX 70, FTIR spectroscopy reveals that Samples have (C=N), (C-O), (M-N) and (M-O) bonds in the range of 4000-400cm{sup −1}. UV-VIS spectroscopy give information that samples absorb the visible light which is in the range of 380-780nm. For this, Lambda 960 spectrometer used. SEM is designed for studying of the solid objects, using JEOL JSM 5600 instrument.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Enabling the Acquisition of Electron Beam-Induced Current (EBIC) Images in Conventional SEM and STEM Instruments

Electron beam-induced current (EBIC) imaging is a well-established scanning electron microscope (SEM) technique used to analyze the behavior of microelectronic devices including solar cells. Recently, the application of EBIC imaging in an aberration-corrected scanning transmission electron microscope (STEM) has been demonstrated and offers great potential for the in situ study of electronic materials, correlating charge transport properties to atomic structural and elemental information. Here, this work presents two ways to implement EBIC imaging in conventional SEM and STEM systems: one relying on the instrument's inherent scanning and imaging electronics and the other involving third-party systems usually available in electron microscopes. The implementation of lock-in EBIC in systems equipped with a fast beam blanker is also described. In addition, this work shows and discusses the different mechanisms at play in EBIC imaging and their dependence on beam energy, sample impedance, and electrical measurement configuration, providing researchers with the basic information needed to apply the technique to their research.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

LIvermore SEM image Tools

Scanning Electron Microscopy (SEM) images provide a variety of structural and morphological information for the characterization of the nanomaterials. This code offers automatic recognition and quantitative analysis of SEM images in a high-throughput manner using computer vision and machine learning techniques. The main function of this application is to extract particle size and morphology information of overlapping nanoparticles and core-shell nanostructures in a user friendly interface. The code is written in C++ with QT environment, and has been tested on MacOSX.

KIM, HYOJIN↗

SEM and STEM X-ray spectrum images

This is supplemental information to a paper tentatively titled Applying Data Analytics Methods to X-ray Spectrum Images. Datasets are in the format of .h5 in the pyUSID flavor. SEM_small.h5 is 5 keV beam energy map of a TiB2 ceramic puck. SEM_large.h5 is a 20 keV map of the same sample. STEM.h5 is a STEM 200 keV map of neutron-irradiated tungsten (due to transmutation burnout, it has become a W-Re-Os alloy).

36 MATERIALS SCIENCE↗

Rapid Evaluation of Particle Properties using Inverse SEM Simulations

This report is the final deliverable of a 3 year project whose purpose was to investigate the possibility of using simulations of X-ray spectra generated inside a scanning electron microscope (SEM) as a means to perform quantitative analysis of the sample imaged in the SEM via an inverse analysis methodology. Using the nine point Technology Readiness Levels (TRL) typically used by the US Department of Defense (DOD) and the National Aeronautics and Space Administration (NASA), this concept is now at a TRL of 3. In other words, this work has proven the feasibility of this concept and is ready to be further investigated to address some of the issues highlighted by this initial proof of concept.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Scanning Electron Microscopy (SEM) Procedure for HE Powders on a LEO 438VP System

This method describes the characterization of HE powders by Scanning Electron Microscopy (SEM). HE particles are dispersed onto an aluminum standard SEM specimen mount. Electron micrographs are collected at various magnifications (150 to 10,000 X) depending on HE particle size.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Scanning Electron Microscopy (SEM) Procedure for HE Powders on a LEO 438VP System

This method describes the characterization of HE powders by Scanning Electron Microscopy (SEM). HE particles are dispersed onto an aluminum standard SEM specimen mount. Electron micrographs are collected at various magnifications (150 to 10,000 X) depending on HE particle size.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Improving Microstructural Quantification in 3D FIB-SEM Tomography

A detailed understanding of 3D microstructural features is crucial during postprocessing of the acquired data, while determining microstructural properties. Focused ion beam and scanning electron microscopy (fib-sem) is an ideal technique for the acquisition and quantification of 3D microstructures in subsurface features. In this work, we evaluated and implemented approaches to quantify 3D morphological features of plutonium oxalate and oxide particles. Image analysis, as well as statistical analysis were utilized to study the effect of process variables on the pore morphology of plutonium oxalate and oxide particles. The primary results were the creation of morphological maps of particles and identify indicators that correlated parameters allowing for discrimination between direct and reverse strike processes. This enabled us to properly quantify and map particles with their images obtained via sem. For this project, the highest correlation was found to be between Volume and Sphericity (R 2 = 0.7432) for the Revere Strike process, and Volume % and Sphericity (R 2 = 0.7450) for the Direct Strike process.

36 MATERIALS SCIENCE↗

SEM analysis of ionizing radiation effects in linear integrated circuits

A successful diagnostic technique was developed using a scanning electron microscope (SEM) as a precision tool to determine ionization effects in integrated circuits. Previous SEM methods radiated the entire semiconductor chip or major areas. The large area exposure methods do not reveal the exact components which are sensitive to radiation. To locate these sensitive components a new method was developed, which consisted in successively irradiating selected components on the device chip with equal doses of electrons /10 to the 6th rad (Si)/, while the whole device was subjected to representative bias conditions. A suitable device parameter was measured in situ after each successive irradiation with the beam off.

Stanley, A. G.↗

Nondestructive SEM for surface and subsurface wafer imaging

The scanning electron microscope (SEM) is considered as a tool for both failure analysis as well as device characterization. A survey is made of various operational SEM modes and their applicability to image processing methods on semiconductor devices.

Propst, Roy H.↗

In-situ thermal cycling in SEM of a graphite-aluminum composite

In situ SEM observations of a graphite-aluminum composite (unidirectional P100 graphite-fiber-reinforced 6061 aluminum MMC plates) were used to measure displacements within the graphite fiber relative to the interface between the graphite fiber and the aluminum matrix during thermal cycling. Specimens were thermally cycled from room temperature to 300 C or 500 C in a SEM chamber and then cooled to room temperature. The obtained shear strains within the fiber were then related to anomalous values of measured residual stresses and to the impact on the composite coefficient of expansion and potential damage under thermal fatigue loading. The shear mechanism was proposed as a source of temperature limits on the low coefficient of expansion of these composites, as well as a potential source of thermal fatigue degradation.

Cheong, Y. M.↗

Payload isolation and stabilization by a Suspended Experiment Mount (SEM)

Many Space Shuttle and Space Station payloads can benefit from isolation from crew or attitude control system disturbances. Preliminary studies have been performed for a Suspended Experiment Mount (SEM) system that will provide isolation from accelerations and stabilize the viewing direction of a payload. The concept consists of a flexible suspension system and payload-mounted control moment gyros. The suspension system, which is rigidly locked for ascent and descent, isolates the payload from high frequency disturbances. The control moment gyros stabilize the payload orientation. The SEM will be useful for payloads that require a lower-g environment than a manned vehicle can provide, such as materials processing, and for payloads that require stabilization of pointing direction, but not large angle slewing, such as nadir-viewing earth observation or solar viewing payloads.

Bailey, Wayne L.↗

Space Experiment Module (SEM)

The Space Experiment Module (SEM) Program is an education initiative sponsored by the National Aeronautics and Space Administration (NASA) Shuttle Small Payloads Project. The program provides nationwide educational access to space for Kindergarten through University level students. The SEM program focuses on the science of zero-gravity and microgravity. Within the program, NASA provides small containers or "modules" for students to fly experiments on the Space Shuttle. The experiments are created, designed, built, and implemented by students with teacher and/or mentor guidance. Student experiment modules are flown in a "carrier" which resides in the cargo bay of the Space Shuttle. The carrier supplies power to, and the means to control and collect data from each experiment.

Brodell, Charles L.↗

SEM Milestone Report for MARMOT Validation Project

MARMOT is a meso-scale fuel code under development by NEAMS designed to predict the microstructure evolution of fuel materials to determine updated thermal and mechanical property models. These updated models can be used by engineering scale codes such as BISON. To support its development and validation the MARMOT Validation Project (MVP) was initiated and consists of extensive microstructure and thermal characterization of U-10Zr fuel material before and at discreet levels of irradiation. This report summarizes the SEM and EDS characterization of the lowest burnup samples (1.5% FIMA) and how they compare to pre-irradiation SEM and EDS.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Towards a quantitative understanding of bonding in supersonic single particle impacts: A three-dimensional FIB-SEM exploration

Particle bonding is crucial to coating quality in cold spray, but it has been a challenge to accurately quantify bonding even in single particle impacts. This paper uses FIB-SEM to explicitly map the particle-substrate interface for Cu-on-Cu single microparticle impacts in a full 3D rendering that spans a wide range of impact velocities. This approach permits a detailed quantification of the total bonding area and all of its associated components. In addition to revealing why prior 2D characterization efforts have missed important details about impact bonding, these data quantitatively reveal the evolution of bonding from its onset at the “critical velocity” V cr (where bonding is generally poor, ∼6 %) to its peak at around 1.3‧V cr (where almost 90 % of the particle bonds). Further increase in the velocity to 1.5‧V cr and beyond finds the onset of hydrodynamic penetration and a decrease in bonding. These data then support the development of a simple analytical model based on oxide rarefication and extrusion of bare metal through gaps in the oxide layer as driving the development of bonding. As a result, the model reproduces the experiments and provides guidance on optimization of bonding as a function of material and process parameters.

Analytical methods↗