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At least 73 records · Page 4

A Miniaturized Variable Pressure Scanning Electron Microscope (MVP-SEM) for In-Situ Mars Surface Sample Analysis

The Miniaturized Variable Pressure Scanning Electron Microscope (MVP-SEM) project, funded by the NASA Planetary Instrument Concepts for the Advancement of Solar System Observations (PICASSO) Research Opportunities in Space and Earth Sciences (ROSES), will build upon previous miniaturized SEM designs and recent advancements in variable pressure SEM's to design and build a SEM to complete analyses of samples on the surface of Mars using the atmosphere as an imaging medium. This project is a collaboration between NASA Marshall Space Flight Center (MSFC), the Jet Propulsion Laboratory (JPL), electron gun and optics manufacturer Applied Physics Technologies, and small vacuum system manufacturer Creare. Dr. Ralph Harvery and environmental SEM (ESEM) inventor Dr. Gerry Danilatos serve as advisors to the team. Variable pressure SEMs allow for fine (nm-scale) resolution imaging and micron-scale chemical study of materials without sample preparation (e.g., carbon or gold coating). Charging of a sample is reduced or eliminated by the gas surrounding the sample. It is this property of ESEMs that make them ideal for locations where sample preparation is not yet feasible, such as the surface of Mars. In addition, the lack of sample preparation needed here will simplify the sample acquisition process and allow caching of the samples for future complementary payload use.

Microscope↗

Dynamic-scanning-electron-microscope study of friction and wear

A friction and wear apparatus was built into a real time scanning electron microscope (SEM). The apparatus and SEM comprise a system which provides the capability of performing dynamic friction and wear experiments in situ. When the system is used in conjunction with dispersive X-ray analysis, a wide range of information on the wearing process can be obtained. The type of wear and variation with speed, load, and time can be investigated. The source, size, and distribution of wear particles can be determined and metallic transferal observed. Some typical results obtained with aluminum, copper, and iron specimens are given.

Brainard, W. A.↗

Examination of Scanning Electron Microscope and Computed Tomography Images of PICA

Micrographs of PICA (Phenolic Impregnated Carbon Ablator) taken using a Scanning Electron Microscope (SEM) and 3D images taken with a Computed Tomography (CT) system are examined. PICA is a carbon fiber based composite (Fiberform ) with a phenolic polymer matrix. The micrographs are taken at different surface depths and at different magnifications in a sample after arc jet testing and show different levels of oxidative removal of the charred matrix (Figs 1 though 13). CT scans, courtesy of Xradia, Inc. of Concord CA, were captured for samples of virgin PICA, charred PICA and raw Fiberform (Fig. 14). We use these images to calculate the thermal conductivity (TC) of these materials using correlation function (CF) methods. CF methods give a mathematical description of how one material is embedded in another and is thus ideally suited for modeling composites like PICA. We will evaluate how the TC of the materials changes as a function of surface depth. This work is in collaboration with ETH-Zurich, which has expertise in high temperature materials and TC modeling (including CF methods).

Lawson, John W.↗

Acquisition of a High Resolution Field Emission Scanning Electron Microscope for the Analysis of Returned Samples

This grant furnished funds to purchase a state-of-the-art scanning electron microscope (SEM) to support our analytical facilities for extraterrestrial samples. After evaluating several instruments, we purchased a JEOL 6500F thermal field emission SEM with the following analytical accessories: EDAX energy-dispersive x-ray analysis system with fully automated control of instrument and sample stage; EDAX LEXS wavelength-dispersive x-ray spectrometer for high sensitivity light-element analysis; EDAX/TSL electron backscatter diffraction (EBSD) system with software for phase identification and crystal orientation mapping; Robinson backscatter electron detector; and an in situ micro-manipulator (Kleindiek). The total price was $550,000 (with $150,000 of the purchase supported by Carnegie institution matching funds). The microscope was delivered in October 2002, and most of the analytical accessories were installed by January 2003. With the exception of the wavelength spectrometer (which has been undergoing design changes) everything is working well and the SEM is in routine use in our laboratory.

Nittler, Larry R.↗

In-Situ Scanning Electron Microscope Experiments for Microscale Mechanical Testing and Validated Modeling of Fiber Reinforced Thermoplastics

A novel, in-situ, scanning electron microscope (SEM) mechanical testing capability for materials at the microscale which provides experimental validation to a machine learning (ML) toolset for full-field validation of physics-based micromechanics models is being developed by researchers at NASA Glenn Research Center. These are enabling technologies for the integration of multiscale digital twins for materials into system level models which will result in the improved performance, material discovery, reduced production cost and time, rapid characterization, and prognostic structural health monitoring (SHM) for materials and structures for extreme environments in support of NASA space exploration missions. In order to bridge the material structure-to-system gap for digital twins, physics-based models must be experimentally validated at multiple length scales. Seminal microscale experiments, conducted at the Air Force Research Laboratory (AFRL), were limited to transverse compression of single-layer, unidirectional thermoset polymer matrix composite (PMC) micropillar specimens [1]. The early phases of the current project followed those initial results and setup to reproduce the compression testing of PMC material on the custom-built piezoelectric actuated micromechanical testing rig built by MicroTesting Solutions LLC. In this work, samples of thermoplastic PMC material were first machined into 3 mm cubes, and then further machining and final milling was done using a Focused Ion Beam (FIB). The initial experiment was done on a pillar roughly 20 µm x 20 µm x 40 µm tall. Additional pillars were milled with final sizes ranging from 20 µm x 20 µm x 40 µm tall to 40 µm x 40 µm x 65 µm tall. A speckle pattern for in-situ full-field measurements using Digital Image Correlation (DIC) was applied with platinum, which was coated on the surface, and then the FIB was used to mill away some of the coating to produce an irregular pattern of Pt on the pillar surface. The samples were loaded into the custom testing rig and placed into the SEM and loaded under compression until failure. Images were collected in the SEM during testing. Post-processing of the images was conducted using DIC to obtain full-field displacement and strain measurements elucidating the role of the matrix as well as fiber-fiber interaction at the microscale within the composite subjected to compression loading well into the non-linear regime of the material. Moreover, the evolution of fiber-matrix debonding and matrix cracking is observed in-situ at the microscale. This data, along with images segmented with a newly developed ML toolset [2], was used to create and validate physics-based micromechanics models. An image of the failed micropillar is shown in Figure 1. The techniques developed in the initial compression experiment was tailored to the validation needs of the models and expanded to include different sized samples as well as possibly tension and fatigue.

Laura Wilson↗

Atomic-Scale Structure and Non-Stoichiometry of Meteoritic Hibonite: A Transmission Electron Microscope Study

Hibonite (CaAl_12O_19) is a common refractory mineral in Ca-Al-rich inclusions (CAIs) in primitive meteorites. Transmission electron microscope (TEM) studies have identified enigmatic planar defects in different occurrences of hibonite in the Allende meteorite that give rise to strong streaking along c* in electron diffraction patterns. Atomic resolution high-angle annular dark-field (HAADF) imaging and energy-dispersive X-ray (EDX) analyses were used to determine the nature and origin of these planar features. HAADF images of hibonite grains reveal lamellar intergrowths of common 1.6 nm spacing, and less commonly 2.0 and 2.5 nm spacings, interspersed in stoichiometric hibonite showing 1.1 nm (002) spacing. Stoichiometric hibonite consists of alternating Ca-containing (“R”) and spinel-structured (“S”) blocks stacked in a sequence RS. In contrast, the 1.6 nm layers result from a doubled S block such that the stacking sequence is RSS, while in the widest defect observed, the stacking sequence is RSSSS. These intergrowths are epitaxial and have coherent, low-strain boundaries with the host hibonite Meteoritic hibonite shows common Ti and Mg substitution for Al in its structure. Atomic-resolution EDX maps of hibonite grains in the Allende CAI confirm the preferred site occupancy of Mg on tetragonal M3 sites in S blocks and of Ti on trigonal bipyramidal M2 and octahedral M4 sites in R blocks. Mg is highly concentrated, but Ti is absent in the planar defects where wider S blocks show Al-rich compositions compared to stoichiometric MgAl_2O_4 spinel. Therefore, Mg likely played the major role in the formation and metastability of planar defects in hibonite. Electron energy loss spectroscopy data from the Ti L_2,3 edge show the presence of mixed Ti oxidation states with ~ 15–20% of Ti as Ti^(3+) in hibonite, suggesting a direct substitution of Ti^(3+) ↔ Al^(3+) in hibonite. The remaining ~ 80–85% of Ti is present as Ti^(4+) and corresponding EDX analyses are consistent with the well-known coupled substitution 2Al^(3+) ↔ Ti^(4+) + Mg^(2+) being the major mechanism for Ti and Mg substitution in hibonite. The formation of planar defects in hibonite occurred during high-temperature nebular condensation or melting/crystallization processes. The occurrence of non-stoichiometric hibonite in the Allende CAI deviates from the mineral formation sequence predicted from equilibrium condensation models. Overall, our atomic resolution TEM observations signify non-equilibrium, kinetic-controlled crystal growth during the high-temperature formation of refractory solids in the early solar nebula.

hibonite↗

A Miniaturized Variable Pressure Scanning Electron Microscope (MVP-SEM) for the Surface of Mars: An Instrument for the Planetary Science Community

The Miniaturized Variable Pressure Scanning Electron Microscope(MVP-SEM) project, funded by the NASA Planetary Instrument Concepts for the Advancement of Solar System Observations (PICASSO) Research Opportunities in Space and Earth Science (ROSES), will build upon previous miniaturized SEM designs for lunar and International Space Station (ISS) applications and recent advancements in variable pressure SEM's to design and build a SEM to complete analyses of samples on the surface of Mars using the atmosphere as an imaging medium. By the end of the PICASSO work, a prototype of the primary proof-of-concept components (i.e., the electron gun, focusing optics and scanning system)will be assembled and preliminary testing in a Mars analog chamber at the Jet Propulsion Laboratory will be completed to partially fulfill Technology Readiness Level to 5 requirements for those components. The team plans to have Secondary Electron Imaging(SEI), Backscattered Electron (BSE) detection, and Energy Dispersive Spectroscopy (EDS) capabilities through the MVP-SEM.

Mars↗

Low energy X-ray spectra measured with a mercuric iodide energy dispersive spectrometer in a scanning electron microscope

A mercuric iodide energy dispersive X-ray spectrometer, with Peltier cooling provided for the detector and input field effect transistor, has been developed and tested in a scanning electron microscope. X-ray spectra were obtained with the 15 keV electron beam. An energy resolution of 225 eV (FWHM) for Mn-K(alpha) at 5.9 keV and 195 eV (FWHM) for the Mg-K line at 1.25 keV has been measured. Overall system noise level was 175 eV (FWHM). The detector system characterization with a carbon target demonstrated good energy sensitivity at low energies and lack of significant spectral artifacts at higher energies.

Iwanczyk, J. S.↗

Determination of bulk diffusion lengths for angle-lapped semiconductor material via the scanning electron microscope: A theoretical analysis

A standard procedure for the determination of the minority carrier diffusion length by means of a scanning electron microscope (SEM) consists in scanning across an angle-lapped surface of a P-N junction and measuring the resultant short circuit current I sub sc as a function of beam position. A detailed analysis of the I sub sc originating from this configuration is presented. It is found that, for a point source excitation, the I sub sc depends very simply on x, the variable distance between the surface and the junction edge. The expression for the I sub sc of a planar junction device is well known. If d, the constant distance between the plane of the surface of the semiconductor and the junction edge in the expression for the I of a planar junction is merely replaced by x, the variable distance of the corresponding angle-lapped junction, an expression results which is correct to within a small fraction of a percent as long as the angle between the surfaces, 2 theta sub 1, is smaller than 10 deg.

Vonroos, O.↗

Miniature Variable Pressure Scanning Electron Microscope for In-Situ Imaging and Chemical Analysis

NASA Marshall Space Flight Center (MSFC) is leading an effort to develop a Miniaturized Variable Pressure Scanning Electron Microscope (MVP-SEM) for in-situ imaging and chemical analysis of uncoated samples. This instrument development will be geared towards operation on Mars and builds on a previous MSFC design of a mini-SEM for the moon (funded through the NASA Planetary Instrument Definition and Development Program). Because Mars has a dramatically different environment than the moon, modifications to the MSFC lunar mini-SEM are necessary. Mainly, the higher atmospheric pressure calls for the use of an electron gun that can operate at High Vacuum, rather than Ultra-High Vacuum. The presence of a CO2-rich atmosphere also allows for the incorporation of a variable pressure system that enables the in-situ analysis of nonconductive geological specimens. Preliminary testing of Mars meteorites in a commercial Environmental SEM(Tradmark) (FEI) confirms the usefulness of lowcurrent/low-accelerating voltage imaging and highlights the advantages of using the Mars atmosphere for environmental imaging. The unique capabilities of the MVP-SEM make it an ideal tool for pursuing key scientific goals of NASA's Flagship Mission Max-C; to perform in-situ science and collect and cache samples in preparation for sample return from Mars.

Gaskin, Jessica A.↗