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NASA NTRS1999

The Mars Environmental Compatibility Assessment (MECA) Abrasion Tool

The Mars Environmental Compatibility Assessment (MECA) experiment, an instrument suite to be flown on Mars Surveyor 2001, will include a tool for doing simple mineralogical scratch and streak tests on particles from the Martian regolith. The Abrasion Tool will be applied to particles that adhere themselves to highly polished substrates of various hardnesses. Granular soil components will be subjected to a compressive force of about 3 N using a leaf spring. The spring will be applied with a paraffin actuator capable of a 0.76 mm throw to achieve a maximum displacement of about 7.5 mm at the tip of the tool. The pressure per grain will be dependent on the grain size, the number of grains that adhere to the substrate and the number of grains in compression. The pressure per particle is expected to be on the order of 100 MPa - 1 GPa. The MECA sample wheel containing the substrates will be rotated after the particles are placed in compression to produce scratches or pits. A primary goal of the Abrasion Tool is to identify quartz (Mohs' hardness = 7) using substrates of varying hardnesses. Quartz is considered hazardous to future human explorers of Mars because it can cause silicosis of the lungs if it is of respirable size. It is also hazardous to machinery, structures, and space suits because of its ability to abrade and scratch surfaces. Since large quantities of minerals harder than quartz are not expected, any scratches produced on polished quartz substrates might be reasonably attributed to quartz particles, although there may be minerals such as impact metamorphic diamond in the soils. Careful calibration of the tool will be necessary to ensure that grains are not overloaded; for example, a steel ball pressed into glass will produce a Hertzian fracture, even though it is softer than glass. Other minerals, such as magnetite (Mohs' hardness = 6.5) have been shown to scratch glass ceramics such as Zerodur (Mohs' hardness = 6.5). Thus, minerals can be differentiated: note that regardless of the mineral species, if any particle is harder than 6.5 it will certainly be an interesting discovery for both planetary geology and human exploration concerns. The scratches will be identified using the 6X optical microscope and profiled with the atomic force microscope included in the MECA instrument suite. Analysis of the scratch morphology will yield evidence concerning the shape of the particle responsible for producing each scratch. For example, angular grains should leave vertical cracks with microconchoidal lateral chipping, while rounded grains might leave chatter marks, or nested partial Hertzian cracks. Particle shape can thus be inferred from these indentation modes, as well as material hardness. In addition, particle size information may also be available if pits caused by rolling particles can be identified. Converse to scratching, the minerals may be crushed at their contact points, and be smeared onto the target substrates to leave what geologists refer to as "streaks". These are cold-welded trails of mineral material that have structure and color indicative of mineral composition. The AFM will determine the morphology of these streaks, while the microscope will ascertain the color. On the harder substrates, we might expect streaking to dominate; on the softer substrates, scratching may dominate. Progressions of material interactions across the substrate selection will be a valuable source of data for mineral discrimination. It should also be noted that many minerals have coatings (such as iron oxides), and these will have to be differentiated from the host mineral grains; laboratory tests will establish the effects of such coatings on the scratch results. Finally, we note that the microscope will provide corroborative data regarding likely mineral species by grain shapes, fracture patterns, surface textures, color, and UV fluorescence reactions. Additional information is contained in the original extended abstract.

Kuhlman, K. R.↗

NASA NTRS1996

Technique to Predict Ultraviolet Radiation Embrittlement of Polymers in Space

In the low-Earth-orbit environment, solar ultraviolet (UV) radiation embrittles polymer materials through bond breaking and crosslinking. This UV embrittlement increases the surface hardness of the polymer. Before the durability of polymer materials in the low- Earth-orbit environment can be predicted, the extent of UV embrittlement needs to be determined. However, traditional techniques for measuring the microhardness of materials cannot be employed to measure changes in the hardness of UV-embrittled surfaces because traditional techniques measure bulk hardness and are not sensitive enough to surface changes. A unique technique was used at the NASA Lewis Research Center to quantify polymer surface damage that had been induced by UV radiation. The technique uses an atomic force microscope (AFM) to measure surface microhardness. An atomic force microscope measures the repulsive forces between the atoms in a microscopic cantilevered tip and the atoms on the surface of a sample. Typically, an atomic force microscope produces a topographic image of a surface by monitoring the movement of the tip over features of the surface. The force applied to the cantilevered tip, and the indention of the tip into the surface, can be measured. The relationship between force and distance of indentation, the quantity force/distance (newtons/meter), provides a measure of the surface hardness. Under identical operating conditions, direct comparisons of surface hardness values can be made.

Source record↗

NASA NTRS2004

Optical Tweezer Assembly and Calibration

An Optical Tweezer, as the name implies, is a useful tool for precision manipulation of micro and nano scale objects. Using the principle of electromagnetic radiation pressure, an optical tweezer employs a tightly focused laser beam to trap and position objects of various shapes and sizes. These devices can trap micrometer and nanometer sized objects. An exciting possibility for optical tweezers is its future potential to manipulate and assemble micro and nano sized sensors. A typical optical tweezer makes use of the following components: laser, mirrors, lenses, a high quality microscope, stage, Charge Coupled Device (CCD) camera, TV monitor and Position Sensitive Detectors (PSDs). The laser wavelength employed is typically in the visible or infrared spectrum. The laser beam is directed via mirrors and lenses into the microscope. It is then tightly focused by a high magnification, high numerical aperture microscope objective into the sample slide, which is mounted on a translating stage. The sample slide contains a sealed, small volume of fluid that the objects are suspended in. The most common objects trapped by optical tweezers are dielectric spheres. When trapped, a sphere will literally snap into and center itself in the laser beam. The PSD s are mounted in such a way to receive the backscatter after the beam has passed through the trap. PSD s used with the Differential Interference Contrast (DIC) technique provide highly precise data. Most optical tweezers employ lasers with power levels ranging from 10 to 100 miliwatts. Typical forces exerted on trapped objects are in the pico-newton range. When PSDs are employed, object movement can be resolved on a nanometer scale in a time range of milliseconds. Such accuracy, however, can only by utilized by calibrating the optical tweezer. Fortunately, an optical tweezer can be modeled accurately as a simple spring. This allows Hook s Law to be used. My goal this summer at NASA Glenn Research Center is the assembly and calibration of an optical tweezer setup in the Instrumentation and Controls Division (5520). I am utilizing a custom LabVIEW Virtual Instrument program for data collection and microscope stage control. Helping me in my assignment are the following people: Mentor Susan Wrbanek (5520), Dr. Baha Jassemnejad (UCO) and Technicians Ken Weiland (7650) and James Williams (7650). Without their help, my task would not be possible.

Collins, Timothy M.↗

NASA NTRS2003

Light Microscopy Module Fan Disturbance Characterized Through Microgravity Emissions Laboratory Testing

A Light Microscopy Module (LMM) is being engineered, designed, and developed at the NASA Glenn Research Center. The LMM is planned as a remotely controllable on-orbit microscope subrack facility, allowing flexible scheduling and control of physical science and biological science experiments within Glenn s Fluids Integrated Rack on the International Space Station. The LMM concept is a modified commercial research imaging light microscope with powerful laser-diagnostic hardware and interfaces, creating a one-of-a-kind, state-of-the-art microscopic research facility. The microscope will house several different objectives, corresponding to magnifications of 10, 40, 50, 63, and 100. Features of the LMM include high-resolution color video microscopy, brightfield, darkfield, phase contrast, differential interference contrast, spectrophotometry, and confocal microscopy combined in a single configuration. Also, laser tweezers are integrated with the diagnostics as a sample manipulation technique. As part of the development phase of the LMM, it was necessary to quantify the microgravity disturbances generated by the control box fan. Isolating the fan was deemed necessary to reduce the fan speed harmonic amplitudes and to eliminate any broadband disturbances across the 60- to 70-Hz and 160- to 170-Hz frequency ranges. The accelerations generated by a control box fan component of the LMM were measured in the Microgravity Emissions Laboratory (MEL). The MEL is a low-frequency measurement system developed to simulate and verify the on-orbit International Space Station (ISS) microgravity environment. The accelerations generated by various operating components of the ISS, if too large, could hinder the science performed onboard by disturbing the microgravity environment. The MEL facility gives customers a test-verified way of measuring their compliance with ISS limitations on vibratory disturbance levels. The facility is unique in that inertial forces in 6 degrees of freedom can be characterized simultaneously for an operating test article. Vibratory disturbance levels are measured for engineering or flight-level hardware following development from component to subassembly through the rack-level configuration. The MEL can measure accelerations as small as 10-7g, the accuracy needed to confirm compliance with ISS requirements.

McNelis, Anne M.↗

NASA NTRS2004

Light Microscopy Module Imaging Tested and Demonstrated

The Fluids Integrated Rack (FIR), a facility-class payload, and the Light Microscopy Module (LMM), a subrack payload, are integrated research facilities that will fly in the U.S. Laboratory module, Destiny, aboard the International Space Station. Both facilities are being engineered, designed, and developed at the NASA Glenn Research Center by Northrop Grumman Information Technology. The FIR is a modular, multiuser scientific research facility that is one of two racks that make up the Fluids and Combustion Facility (the other being the Combustion Integrated Rack). The FIR has a large volume dedicated for experimental hardware; easily reconfigurable diagnostics, power, and data systems that allow for unique experiment configurations; and customizable software. The FIR will also provide imagers, light sources, power management and control, command and data handling for facility and experiment hardware, and data processing and storage. The first payload in the FIR will be the LMM. The LMM integrated with the FIR is a remotely controllable, automated, on-orbit microscope subrack facility, with key diagnostic capabilities for meeting science requirements--including video microscopy to observe microscopic phenonema and dynamic interactions, interferometry to make thin-film measurements with nanometer resolution, laser tweezers to manipulate micrometer-sized particles, confocal microscopy to provide enhanced three-dimensional visualization of structures, and spectrophotometry to measure the photonic properties of materials. Vibration disturbances were identified early in the LMM development phase as a high risk for contaminating the science microgravity environment. An integrated FIR-LMM test was conducted in Glenn's Acoustics Test Laboratory to assess mechanical sources of vibration and their impact to microscopic imaging. The primary purpose of the test was to characterize the LMM response at the sample location, the x-y stage within the microscope, to vibration emissions from the FIR and LMM support structures.

Gati, Frank↗

NASA NTRS2008

Cell-Detection Technique for Automated Patch Clamping

A unique and customizable machinevision and image-data-processing technique has been developed for use in automated identification of cells that are optimal for patch clamping. [Patch clamping (in which patch electrodes are pressed against cell membranes) is an electrophysiological technique widely applied for the study of ion channels, and of membrane proteins that regulate the flow of ions across the membranes. Patch clamping is used in many biological research fields such as neurobiology, pharmacology, and molecular biology.] While there exist several hardware techniques for automated patch clamping of cells, very few of those techniques incorporate machine vision for locating cells that are ideal subjects for patch clamping. In contrast, the present technique is embodied in a machine-vision algorithm that, in practical application, enables the user to identify good and bad cells for patch clamping in an image captured by a charge-coupled-device (CCD) camera attached to a microscope, within a processing time of one second. Hence, the present technique can save time, thereby increasing efficiency and reducing cost. The present technique involves the utilization of cell-feature metrics to accurately make decisions on the degree to which individual cells are "good" or "bad" candidates for patch clamping. These metrics include position coordinates (x,y) in the image plane, major-axis length, minor-axis length, area, elongation, roundness, smoothness, angle of orientation, and degree of inclusion in the field of view. The present technique does not require any special hardware beyond commercially available, off-the-shelf patch-clamping hardware: A standard patchclamping microscope system with an attached CCD camera, a personal computer with an imagedata- processing board, and some experience in utilizing imagedata- processing software are all that are needed. A cell image is first captured by the microscope CCD camera and image-data-processing board, then the image data are analyzed by software that implements the present machine-vision technique. This analysis results in the identification of cells that are "good" candidates for patch clamping (see figure). Once a "good" cell is identified, a patch clamp can be effected by an automated patchclamping apparatus or by a human operator. This technique has been shown to enable reliable identification of "good" and "bad" candidate cells for patch clamping. The ultimate goal in further development of this technique is to combine artificial-intelligence processing with instrumentation and controls in order to produce a complete "turnkey" automated patch-clamping system capable of accurately and reliably patch clamping cells with a minimum intervention by a human operator. Moreover, this technique can be adapted to virtually any cellular-analysis procedure that includes repetitive operation of microscope hardware by a human.

McDowell, Mark↗

NASA NTRS2010

Multiparallel Three-Dimensional Optical Microscopy

Multiparallel three-dimensional optical microscopy is a method of forming an approximate three-dimensional image of a microscope sample as a collection of images from different depths through the sample. The imaging apparatus includes a single microscope plus an assembly of beam splitters and mirrors that divide the output of the microscope into multiple channels. An imaging array of photodetectors in each channel is located at a different distance along the optical path from the microscope, corresponding to a focal plane at a different depth within the sample. The optical path leading to each photodetector array also includes lenses to compensate for the variation of magnification with distance so that the images ultimately formed on all the photodetector arrays are of the same magnification. The use of optical components common to multiple channels in a simple geometry makes it possible to obtain high light-transmission efficiency with an optically and mechanically simple assembly. In addition, because images can be read out simultaneously from all the photodetector arrays, the apparatus can support three-dimensional imaging at a high scanning rate.

Nguyen, Lam K.↗

NASA NTRS2005

Radiation Dosimetry via Automated Fluorescence Microscopy

A developmental instrument for assessment of radiation-induced damage in human lymphocytes includes an automated fluorescence microscope equipped with a one or more chargecoupled- device (CCD) video camera(s) and circuitry to digitize the video output. The microscope is also equipped with a three-axis translation stage that includes a rotation stage, and a rotary tray that holds as many as thirty specimen slides. The figure depicts one version of the instrument. Once the slides have been prepared and loaded into the tray, the instrument can operate unattended. A computer controls the operation of the stage, tray, and microscope, and processes the digital fluorescence-image data to recognize and count chromosomes that have been broken, presumably by radiation. The design and method of operation of the instrument exploit fluorescence in situ hybridization (FISH) of metaphase chromosome spreads, which is a technique that has been found to be valuable for monitoring the radiation dose to circulating lymphocytes. In the specific FISH protocol used to prepare specimens for this instrument, metaphase lymphocyte cultures are chosen for high mitotic index and highly condensed chromosomes, then several of the largest chromosomes are labeled with three of four differently colored whole-chromosome-staining dyes. The three dyes, which are used both individually and in various combinations, are fluorescein isothiocyanate (FITC), Texas Red (or equivalent), and Cy5 (or equivalent); The fourth dye 4',6-diamidino- 2-phenylindole (DAPI) is used as a counterstain. Under control by the computer, the microscope is automatically focused on the cells and each slide is scanned while the computer analyzes the DAPI-fluorescence images to find the metaphases. Each metaphase field is recentered in the field of view and refocused. Then a four-color image (more precisely, a set of images of the same view in the fluorescent colors of the four dyes) is acquired. By use of pattern-recognition software developed specifically for this instrument, the images in the various colors are processed to recognize the metaphases and count the chromosome fragments of each color within the metaphases. The intermediate results are then further processed to estimate the proportion of cells that have suffered genetic damage. The prototype instrument scans at an average areal rate of 4.7 mm2/h in unattended operation, finding about 14 metaphases per hour. The false-alarm rate is typically less than 3 percent, and the metaphase-miss rate has been estimated to be less than 5 percent. The counts of chromosomes and fragments thereof are 50 to 70 percent accurate.

Castleman, Kenneth R.↗

NASA NTRS2004

Compact, Automated Centrifugal Slide-Staining System

The Directional Acceleration Vector-Driven Displacement of Fluids (DAVD-DOF) system, under development at the time of reporting the information for this article, would be a relatively compact, automated, centrifugally actuated system for staining blood smears and other microbiological samples on glass microscope slides in either a microgravitational or a normal Earth gravitational environment. The DAVD-DOF concept is a successor to the centrifuge-operated slide stainer (COSS) concept, which was reported in Slide-Staining System for Microgravity or Gravity (MSC-22949), NASA Tech Briefs, Vol. 25, No. 1 (January, 2001), page 64. The COSS includes reservoirs and a staining chamber that contains a microscope slide to which a biological sample is affixed. The staining chamber is sequentially filled with and drained of staining and related liquids from the reservoirs by use of a weighted plunger to force liquid from one reservoir to another at a constant level of hypergravity maintained in a standard swing-bucket centrifuge. In the DAVD-DOF system, a staining chamber containing a sample would also be sequentially filled and emptied, but with important differences. Instead of a simple microscope slide, one would use a special microscope slide on which would be fabricated a network of very small reservoirs and narrow channels connected to a staining chamber (see figure). Unlike in the COSS, displacement of liquid would be effected by use of the weight of the liquid itself, rather than the weight of a plunger.

Feeback, Daniel L.↗

NASA NTRS2012

Metrology of Large Parts

As discussed in the first chapter of this book, there are many different methods to measure a part using optical technology. Chapter 2 discussed the use of machine vision to measure macroscopic features such as length and position, which was extended to the use of interferometry as a linear measurement tool in chapter 3, and laser or other trackers to find the relation of key points on large parts in chapter 4. This chapter looks at measuring large parts to optical tolerances in the sub-micron range using interferometry, ranging, and optical tools discussed in the previous chapters. The purpose of this chapter is not to discuss specific metrology tools (such as interferometers or gauges), but to describe a systems engineering approach to testing large parts. Issues such as material warpage and temperature drifts that may be insignificant when measuring a part to micron levels under a microscope, as will be discussed in later chapters, can prove to be very important when making the same measurement over a larger part. In this chapter, we will define a set of guiding principles for successfully overcoming these challenges and illustrate the application of these principles with real world examples. While these examples are drawn from specific large optical testing applications, they inform the problems associated with testing any large part to optical tolerances. Manufacturing today relies on micrometer level part performance. Fields such as energy and transportation are demanding higher tolerances to provide increased efficiencies and fuel savings. By looking at how the optics industry approaches sub-micrometer metrology, one can gain a better understanding of the metrology challenges for any larger part specified to micrometer tolerances. Testing large parts, whether optical components or precision structures, to optical tolerances is just like testing small parts, only harder. Identical with what one does for small parts, a metrologist tests large parts and optics in particular to quantify their mechanical properties (such as dimensions, mass, etc); their optical prescription or design (i.e. radius of curvature, conic constant, vertex location, size); and their full part shape. And, just as with small parts, a metrologist accomplishes these tests using distance measuring instruments such as tape measures, inside micrometers, coordinate measuring machines, distance measuring interferometers; angle measuring instruments such as theodolites, autocollimators; and surface measuring instruments including interferometers, stylus profilers, interference microscopes, photogrammetric cameras, or other tools. However, while the methodology may be similar, it is more difficult to test a large object for the simple reason that most metrologists do not have the necessary intuition. The skills used to test small parts or optics in a laboratory do not extrapolate to testing large parts in an industrial setting any more than a backyard gardener might successfully operate a farm. But first, what is a large part? A simple definition might be the part's size or diameter. For optics and diffuse surface parts alike, the driving constraint is ability to illuminate the part's surface. For reflective convex mirrors, large is typically anything greater than 1 meter. But, for refractive optics, flats or convex mirrors, large is typically greater than 0.5 meter. While a size definition is simple, it may be less than universal. A more nuanced definition might be that a large part is any component which cannot be easily tested in a standard laboratory environment, on a standard vibration isolated table using standard laboratory infrastructure. A micro-switch or a precision lens might be easily measured to nanometer levels under a microscope in a lab, but a power turbine spline or a larger telescope mirror will not fit under that microscope and may not even fit on the table.

Stahl, H. Philip↗

NASA NTRS2007

KLASS: Kennedy Launch Academy Simulation System

Software provides access to many sophisticated scientific instrumentation (Scanning Electron Microscope (SEM), a Light Microscope, a Scanning Probe Microscope (covering Scanning Tunneling, Atomic Force, and Magnetic Force microscopy), and an Energy Dispersive Spectrometer for the SEM). Flash animation videos explain how each of the instruments work. Videos on how they are used at NASA and the sample preparation. Measuring and labeling tools provided with each instrument. Hands on experience of controlling the virtual instrument to conduct investigations, much like the real scientists at NASA do. Very open architecture. Open source on SourceForge. Extensive use of XML Target audience is high school and entry-level college students. "Many beginning students never get closer to an electron microscope than the photos in their textbooks. But anyone can get a sense of what the instrument can do by downloading this simulator from NASA's Kennedy Space Center." Science Magazine, April 8th, 2005

Garner, Lesley C.↗

NASA NTRS2014

A Novel Protocol for Decoating and Permeabilizing Bacterial Spores for Epifluorescent Microscopy

Based on previously reported procedures for permeabilizing vegetative bacterial cells, and numerous trial-and-error attempts with bacterial endospores, a protocol was developed for effectively permeabilizing bacterial spores, which facilitated the applicability of fluorescent in situ hybridization (FISH) microscopy. Bacterial endospores were first purified from overgrown, sporulated suspensions of B. pumilus SAFR-032. Purified spores at a concentration of approx equals 10 million spores/mL then underwent proteinase-K treatment, in a solution of 468.5 μL of 100 mM Tris-HCl, 30 μL of 10% SDS, and 1.5 microL of 20 mg/mL proteinase-K for ten minutes at 35 ºC. Spores were then harvested by centrifugation (15,000 g for 15 minutes) and washed twice with sterile phosphate-buffered saline (PBS) solution. This washing process consisted of resuspending the spore pellets in 0.5 mL of PBS, vortexing momentarily, and harvesting again by centrifugation. Treated and washed spore pellets were then resuspended in 0.5 mL of decoating solution, which consisted of 4.8 g urea, 3 mL Milli-Q water, 1 mL 0.5M Tris, 1 mL 1M dithiothreitol (DTT), and 2 mL 10% sodium-dodecylsulfate (SDS), and were incubated at 65 ºC for 15 minutes while being shaken at 165 rpm. Decoated spores were then, once again, washed twice with sterile PBS, and subjected to lysozyme/mutanolysin treatment (7 mg/mL lysozyme and 7U mutanolysin) for 15 minutes at 35 C. Spores were again washed twice with sterile PBS, and spore pellets were resuspended in 1-mL of 2% SDS. This treatment, facilitating inner membrane permeabilization, lasted for ten minutes at room temperature. Permeabilized spores were washed two final times with PBS, and were resuspended in 200 mkcroL of sterile PBS. At this point, the spores were permeable and ready for downstream processing, such as oligonucleotideprobe infiltration, hybridization, and microscopic evaluation. FISH-microscopic imagery confirmed the effective and efficient (≈50% successful permeabilization and recovery) permeabilization of numerous spore preparations. The novelty of the technology developed here is in its applicability to bacterial endospores. While protocols abound for the effective permeabilization of bacterial, archaeal, and eukaryotic vegetative cells, there are no such reliable methods for decoating and permeabilizing bacterial endospores in a manner that is amenable to downstream FISH microscopic analyses. This innovation enables the direct visualization and enumeration of spores via FISH-based microscopic techniques, circumventing the complications that accompany previously required germination regimes. The synergistic enzymatic weakening of the many spore layers facilitates a structural compromise that is just enough to render the spores permeable without degrading the spore to a level, which precludes it from recognition.

LaDuc, Myron T.↗

NASA NTRSDate not supplied

A General Model for the Electrochemical Double Layer in Solids

It has long been clear that electrochemical double layer / space charge zone in the vicinity of interfaces and other extended defects greatly influences transport and reactivity. Over the past several years, multiple microscopic measurements of defect concentrations in the vicinity of solid-solid interfaces made clear that dilute-case thermodynamic theories to describe the behavior of charged species in space charge zones are untenable. Inhomogeneous thermodynamics – i.e., phase field models – have delivered the most success in describing both microscopic and macroscopic experiments. We still need a generalized approach that quantitatively reproduces the microscopic and macroscopic evidence, while remaining accessible to a wide range of researchers and engineers. In my talk I will present such a framework, which builds on the previously introduced Poisson-Cahn theory but utilizes data science methods which come into the thermodynamic framework in a well-defined way. I will review recent applications to both microscopic and macroscopic datasets while previewing our plans for connecting the theory to atomistic / first principles calculations and experiment simultaneously. I will also review plans for releasing open source code that runs on desktop-level computational resources.

David Mebane↗

NASA NTRSDate not supplied

Variable Pressure - Scanning Electron Microscopy (VP-SEM)

Variable Pressure (or Environmental) Scanning Electron Microscopy (VP-SEM) combined with Energy Dispersive X-ray Spectroscopy (EDS) is one of the most powerful methods for characterizing the sub-micron topography and chemical composition of uncoated samples. Terrestrially, VP-SEM is extensively used to non-destructively study geologic and manufactured materials with high spatial resolution (tens of nanometers) and large depth-of-field. An SEM offers a geologist a first survey of microscopic mineral phases via secondary electron imaging (SEI), which provides a topographic look at a sample, as well as backscattered electron (BEI) imaging, which contrasts the phases present based on their geochemistry (atomic number). A VP-SEM utilizes a gas in the sample chamber as a charge dissipation and signal amplification method, allowing analysis of a sample without preparation in the form of a conductive coating. A miniaturized VP-SEM operating in-situ on a lander or rover would be able to use the CO2-rich Martian atmosphere (e.g., Nier et al., 1976; Williams 2016) as an imaging medium for this purpose. Adaptation of a VP-SEM for in-situ Mars surface studies will provide a new imaging capability (via SEI) that is at least an order of magnitude higher resolution than the Mars Hand Lens Imager (MAHLI) on the Mars Science Laboratory (Williams et al., 2015), and equal to or better than the achieved resolution of the Atomic Force Microscope on the Phoenix Mars lander (Pike et al., 2011). In addition, the MVP-SEM is capable of BSI and simultaneous chemical analysis of the imaged region. In this sense, the MVP-SEM can be regarded as an instrument suite that will provide a new set of information not achievable by any other instrument. The Miniaturized Variable Pressure Scanning Electron Microscope (MVP-SEM) was designed, built, and benchtop tested by a team at NASA’s Marshall Space Flight Center and Jet Propulsion Laboratory (JPL), Jacobs Space Exploration Group, Applied Physics Technologies, Inc. (AP-Tech), and Creare LLC, working with a team of technical and science collaborators. Benchtop testing was successful, proving concept feasibility. To date, the MVP-SEM has achieved an imaging resolution of <100 nm in the lab, and with continued optimization, even better performance (~50 nm resolution) is possible. Use in-situ on the lunar or other planetary surfaces would require some redesign to optimize instrument performance, but such an instrument would be equally useful.

Variable Pressure Scanning Electron Microscopy↗

NASA NTRSDate not supplied

Miniature Variable Pressure - Scanning Electron Microscopy (MVP-SEM)

Variable Pressure Scanning Electron Microscopy↗

DOE OSTI2024

AEcroscopy: A Software–Hardware Framework Empowering Microscopy Toward Automated and Autonomous Experimentation

Microscopy has been pivotal in improving the understanding of structure-function relationships at the nanoscale and is by now ubiquitous in most characterization labs. However, traditional microscopy operations are still limited largely by a human-centric click-and-go paradigm utilizing vendor-provided software, which limits the scope, utility, efficiency, effectiveness, and at times reproducibility of microscopy experiments. Here, in this work, a coupled software–hardware platform is developed that consists of a software package termed AEcroscopy (short for Automated Experiments in Microscopy), along with a field-programmable-gate-array device with LabView-built customized acquisition scripts, which overcome these limitations and provide the necessary abstractions toward full automation of microscopy platforms. The platform works across multiple vendor devices on scanning probe microscopes and electron microscopes. It enables customized scan trajectories, processing functions that can be triggered locally or remotely on processing servers, user-defined excitation waveforms, standardization of data models, and completely seamless operation through simple Python commands to enable a plethora of microscopy experiments to be performed in a reproducible, automated manner. This platform can be readily coupled with existing machine-learning libraries and simulations, to provide automated decision-making and active theory-experiment optimization to turn microscopes from characterization tools to instruments capable of autonomous model refinement and physics discovery.

47 OTHER INSTRUMENTATION↗

DOE OSTI2026

Nonlocal Effect of Percolated Particle Networks on Viscoelasticity of Polymer–Filler Nanocomposites: A Mesoscale Simulation Study

With nanoparticles (NPs) as fillers, polymer nanocomposites (PNCs) usually exhibit enhanced mechanical properties. However, a direct connection between the microscopic structural relaxation and macroscopic mechanical properties of PNCs remains to be established. To investigate the micro-to-macro connection, we develop a mesoscale model, in which the NPbridging polymer chains are represented by a dynamic bonded interaction between NPs, and the bulk polymer matrix is implicitly modeled by overdamped Langevin dynamics. Extensive equilibrium simulations are performed to quantify the microscopic dynamics of model PNCs. Systematic analyses of modified Rouse dynamics, dynamic structure factor, and relaxation modulus uncover that the microscopic relaxation dynamics of PNCs are significantly decelerated across different length scales because of nonlocal effects of percolated particle networks a phenomenon that has not been adequately captured in prior simulation studies. We find that NPvolume- fraction and NP-bonding-energy barrier are the two critical variables that affect bulk viscoelasticity the most. The proposed mesoscale model is versatile and provides a powerful framework for studying structure−property relations of different PNCs.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2026

Deep generative learning of magnetic frustration in artificial spin ice from magnetic force microscopy images

Increasingly large datasets of microscopic images with nanoscale resolution facilitate the development of machine learning methods to identify and analyze subtle physical phenomena embedded within the images. In this work, microscopic images of honeycomb lattice spin-ice samples serve as datasets from which we automate the calculation of net magnetic moments and directional orientations of spin-ice configurations. In the first stage of our workflow, machine learning models are trained to accurately predict magnetic moments and directions within spin-ice structures. Variational Autoencoders (VAEs), an emergent unsupervised deep learning technique, are employed to generate high-quality synthetic magnetic force microscopy (MFM) images and extract latent feature representations, thereby reducing experimental and segmentation errors. The second stage of proposed methodology enables precise identification and prediction of frustrated vertices and nanomagnetic segments, effectively correlating structural and functional aspects of microscopic images. This facilitates the design of optimized spin-ice configurations with controlled frustration patterns, enabling potential on-demand synthesis.

36 MATERIALS SCIENCE↗