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Optical Scattering Characterization for the Glennan Microsystems Microscale Particulate Classifier

Small sensors that are tolerant to mechanically and thermally harsh environments present the possibility for in-situ particle characterization in propulsion, industrial, and planetary science applications. Under a continuing grant from the Glennan Microsystems Initiative to the Microgravity Fluids Physics Branch of the NASA-Glenn Research Center, a Microscale Particle Classifier (MiPAC) instrument is being developed. The MiPAC instrument will be capable of determining the size distribution of airborne particles from about 1 nm to 30 micrometers, and will provide partial information as to the concentration, charge state, shape, and structure of the particles, while being an order of magnitude smaller in size and lighter in weight than presently commercially available instruments. The portion of the instrument that will characterize the nm-range particles will employ electrical mobility techniques and is being developed under a separate grant to Prof. David Pui of the University of Minnesota. The portion of the instrument that will characterize the micrometer-size particles such as dirt, pollens, spores, molds, soot, and combustion aerosols will use light scattering techniques. The development of data analysis techniques to be employed in the light scattering portion of the instrument is covered by this grant.

Lock, James A.

Microscale Distribution of Hydrogen Isotopes in Two Carbonaceous Chondrites

Hydrogen isotopes are highly variable among primitive meteorites and interplanetary dust particles (IDPs) [1, 2]. In particular, many primitive objects exhibit D (and N-15) enrichments, relative to terrestrial values, thought to represent partial preservation of presolar material fractionated in molecular clouds. However, the diversity of D/H ratios among IDPs and chondrites indicates a complex history of processing in the solar nebula and on meteorite parent bodies. Deconvolving this record requires identification and characterization of the carriers of D enrichments in different objects. Isotopic imaging has proven to be a powerful method to quantitatively explore the distribution of D/H ratios on a one to several m scale in IDPs [2-4] and the CR chondrite Renazzo [5, 6]. In this study, we have used ion imaging to explore the microscale D/H distribution of two carbonaceous chondrites, Tagish Lake (unique) and Al Rais (CR2). Previous D/H measurements (on a ~tens of microns scale) of Tagish Lake matrix fragments by Messenger [7] and Engrand et al. [8] have found different results, most likely related to the analytical techniques used. Previous work has also shown a large range of D/H ratios in CR chondrites, including very large variations on a scale of a few microns [5, 6, 9].

Young, A. F.

Microscale Particulate Classifiers (MiPAC) Being Developed

The NASA Glenn Research Center is developing microscale sensors to characterize atmospheric-borne particulates. The devices are fabricated using MEMS (microelectromechanical systems) technologies. These technologies are derived from those originally developed in support of the semiconductor processing industry. The resulting microsensors can characterize a wide range of particles and are, therefore, suitable to a broad range of applications. This project is supported under a collaborative program called the Glennan Microsystems Initiative. The initiative comprises members of NASA Glenn Research Center, various university affiliates from the State of Ohio, and a number of participating industrial partners. Funding is jointly provided by NASA, the State of Ohio, and industrial members. The work described here is a collaborative arrangement between researchers at Glenn, the University of Minnesota, The National Institute of Standards and Technology (NIST), and the Cleveland State University. Actual device fabrication is conducted at Glenn and at the laboratories of Case Western Reserve University. Case Western is also located in Cleveland, Ohio, and is a participating member of the initiative. The principal investigator for this project is Paul S. Greenberg of Glenn. Two basic types of devices are being developed, and target different ranges of particle sizes. The first class of devices, which is used to measure nanoparticles (i.e., particles in the range of 0.002 to 1 mm), is based on the technique of Electrical Mobility Classification. This technique also affords the valuable ability of measuring the electrical charge state of the particles. Such information is important in the understanding of agglomeration mechanisms and is useful in the development of methods for particle repulsion. The second type of device being developed, which utilizes optical scattering, is suitable for particles larger than 1 mm. This technique also provides information on particle shape and composition. Applications for these sensors include fundamental planetary climatology, monitoring and filtration in spacecraft, human habitation modules and related systems, characterization of particulate emissions from propulsion and power systems, and as early warning sensors for both space-based and ter-restrial fire detection. These devices are also suitable for characterizing biological compounds such as allergens, infectious agents, and biotoxic agents.

Greenberg, Paul S.

Microscale out-of-plane anemometer

A microscale out-of-plane thermal sensor. A resistive heater is suspended over a substrate by supports raised with respect to the substrate to provide a clearance underneath the resistive heater for fluid flow. A preferred fabrication process for the thermal sensor uses surface micromachining and a three-dimensional assembly to raise the supports and lift the resistive heater over the substrate.

Liu, Chang

Using PEACE Data from the four CLUSTER Spacecraft to Measure Compressibility, Vorticity, and the Taylor Microscale in the Magnetosheath and Plasma Sheet

We present determinations of compressibility and vorticity in the magnetosheath and plasma sheet using moments from the four PEACE thermal electron instruments on CLUSTER. The methodology used assumes a linear variation of the moments throughout the volume defined by the four satellites, which allows spatially independent estimates of the divergence, curl, and gradient. Once the vorticity has been computed, it is possible to estimate directly the Taylor microscale. We have shown previously that the technique works well in the solar wind. Because the background flow speed in the magnetosheath and plasma sheet is usually less than the Alfven speed, the Taylor frozen-in-flow approximation cannot be used. Consequently, this four spacecraft approach is the only viable method for obtaining the wave number properties of the ambient fluctuations. Our results using electron velocity moments will be compared with previous work using magnetometer data from the FGM experiment on Cluster.

Goldstein, Melvyn L.

Method for fabricating a microscale anemometer

Method for fabricating a microscale anemometer on a substrate. A sacrificial layer is formed on the substrate, and a metal thin film is patterned to form a sensing element. At least one support for the sensing element is patterned. The sacrificial layer is removed, and the sensing element is lifted away from the substrate by raising the supports, thus creating a clearance between the sensing element and the substrate to allow fluid flow between the sensing element and the substrate. The supports are raised preferably by use of a magnetic field applied to magnetic material patterned on the supports.

Liu, Chang

Evaluation of the Anisotropic Radiative Conductivity of a Low-Density Carbon Fiber Material from Realistic Microscale Imaging

The radiative heat transfer inside a low-density carbon fiber insulator is analyzed using a three-dimensional direct simulation model. A robust procedure is presented for the numerical calculation of the geometric configuration factor to compute the radiative energy exchange processes among the small discretized surface areas of the fibrous material. The methodology is applied to a polygonal mesh of a fibrous insulator obtained from three-dimensional microscale imaging of the real material. The anisotropic values of the radiative conductivity are calculated for that geometry. The results yield both directional and thermal dependence of the radiative conductivity.

Evaluation

Microscale Analysis of Spacecraft Heat Shields

Imagine entering Earth’s atmosphere after returning from the outer solar system. A heat shield less than 2 inches thick protects you from temperatures up to 2,900° Celsius (5,252° Fahrenheit). Such conditions were experienced by NASA’s Stardust capsule during reentry in 2006. The only materials capable of providing the necessary protection are composites with complex microstructures. Evaluating these materials is difficult, requiring precise knowledge of their properties. To this end, NASA scientists are developing research codes to compute material properties and simulate ablation at the microscale using agency supercomputers. Utilizing these tools, along with experiments, researchers are working to push the limits of spaceflight, allowing for greater flexibility in future space missions.

Thornton, John M.

Microscale Characterization of Damage Accumulation in CMCs

The developing roles of damage mechanisms in the failure response of SiC/SiC minicomposites was investigated by the characterization of microscale damage accumulation with respect to microstructure. A multi-modal approach combining spatially resolved acoustic emission (AE) with tensile testing in-SEM (scanning electron microscope) was used to simultaneously examine surface (observed in-SEM) and bulk damage (monitored via AE). Strong agreement was shown between the evolving crack density estimated by AE and in-SEM measurements. The following were observed: (i) in-plane matrix content and distribution impacted crack growth; (ii) spatially-distributed matrix cracks generated varying stress-dependent AE; and (iii) certain individual cracks became more probable failure locations due to unique combinations of damage mechanisms that drove their growth. This approach enabled characterizing potential failure determinants and suggests that early damage behavior is related to certain microstructural features (e.g. surface flaws), while subsequent damage behavior is coupled to interactions of local mechanisms evolving with stress.

ceramic matrix composites

Bridging the Gap Between Microscale Modeling and Additive Manufacturing for TPS

An overview of the now open-source NASA ARC software PuMA will be provided. On top of the well-documented ability to import and compute material properties from micro-CT images, PuMA has the ability to design microstructures and compute/predict material properties such as: porosity, permeability, tortuosity, thermal and electrical conductivity, tensile strength, etc. Therefore, a whole new range of capabilities is available, and provides users with the ability to build TPS materials (both fibrous and woven types) and optimize their properties based on missions and requirements. This talk will aim to provide a seed to start bridging the gap between microscale modeling of TPS materials and additive manufacturing.

Conductivity

Observing Coronal Microscales and Their Connection With Mesoscales

Why the Sun has a tenuous upper atmosphere some 1000 times hotter than the photosphere is a fundamental open problem in space plasma physics despite decades of study. A leading hypothesis, supported by indirect evidence, is that in most of the corona heating is confined to narrow current sheets in which energy is dissipated despite the low large-scale resistivity of the coronal plasma. Although the kinetic scales of reconnection or wave heating are beyond remote observation, thermal structure on scales ≲100 km are expected to be produced by the primary heating mechanisms operating within a filamentary magnetic field. This white paper considers what could be learned from direct observations of coronal plasma on those scales and outlines a mission concept that is more fully described in a Heliophysics Mission Concept Study for the Coronal Microscale Observatory.

Douglas Rabin

Microscale Metal Additive Manufacturing by Solid‐State Impact Bonding of Shaped Thin Films

The deposition of device-grade inorganic materials is one key challenge toward the implementation of additive manufacturing (AM) in microfabrication, and to that end, a broad range of physico-chemical principles has been explored for 3D fabrication with micro- and nanoscale resolution. Yet, for metals, a process that achieves material quality rivalling that of established thin-film deposition methods, and at the same time, has the potential to combine high throughput production with a broad palette of processable materials, is still lacking. Here, the kinetic, solid-state bonding of metal thin films for the additive assembly of high-purity, high-density metals with micrometer-scale precision is introduced. Indirect laser ablation accelerates micrometer-thick gold films to hundreds of meters per second without their heating or ablation. Their subsequent impact on the substrate above a critical velocity forms a permanent, metallic bond in the solid state. Stacked layers are of high density (>99%). By defining thin-film layers with established lithographic methods prior to launch, a variable feature size (2–50 µm), arbitrary shape of bonded layers, and parallel transfer of up to 36 independent film units in a single shot, is demonstrated. Thus, the solid-state kinetic bonding principle as a viable and potentially versatile route for micro-scale AM of metals is established.

3D printing

Root size and soil physicochemical properties drive microscale spatial patterns of Fe and As retention in the rice rhizosphere

Background and Aims: Radial oxygen loss from rice roots in flooded soils oxidizes and precipitates dissolved Fe(II), Mn(II), and As(III) into mixed Fe(III), Mn(III/IV), and As(V) as root plaque and in the rhizosphere soil. It is unknown how different soils and root sizes impact the spatial extent of Fe and As retention outside the root. Methods: We imaged cross-sections of 90 roots from 6 different soils using synchrotron μXRF imaging followed by k-means clustering and elliptical averaging to distinguish bulk soil, rhizosphere, plaque, and roots based on As and Fe patterns. Results: We found preferential As retention in the plaque and rhizospheres of most roots except small (< 0.45 mm) roots in silty soils with low P or high As. In contrast, clayey soils had similar As-Fe correlations across plaque, rhizosphere, and bulk soil. Large (> 0.45 mm) roots often had no oxidized rhizosphere region. We obtained an extensive dataset of 256 As and 155 Mn synchrotron μXANES measurements, which revealed that rhizosphere and plaque As was mainly inorganic As(V) and As(III), and Mn oxidation state varied between soils but not between belowground locations. Conclusion: Small roots in coarse-textured soils were less likely to have As retention in the plaque or rhizosphere compared to large roots and fine-textured soils. Furthermore, the unique and extensive data in this study provides new insight into soil and root size impacts on As retention in the rhizosphere. It is essential to investigate a representative number of samples to draw conclusions from XRF imaging.

36 MATERIALS SCIENCE

Statistical evaluation of microscale stress conditions leading to void nucleation in the weak shock regime

Here, we investigate the heterogeneity of the stress state driven by anisotropic deformation response at the single crystal level through five statistical volume element (SVE) calculations of polycrystalline BCC tantalum. This work focuses on grain boundaries as a prominent material defect type prone to void nucleation based upon experimental observations of predominantly intergranular void nucleation in this material. The SVEs are constructed to be statistically representative of larger volumes of material and are meshed such that mean and standard deviation of grain size and orientation information is reconstructed. The computational meshes feature hexahedral (brick) elements and smooth conformal grain boundaries where significant stress concentration is known to occur, a tail effect of interest in the extreme events process of dynamic ductile damage. An existing micromechanical crystallographic plasticity model shown to capture the single crystal behavior of BCC tantalum well is used to perform the polycrystal calculations. The model includes representation of the non-Schmid effect of non-planar screw dislocation kinetics in tantalum. A three-dimensional stress state time profile predicted by damage modeling of a flyer plate impact experiment is applied as boundary conditions to each SVE. Resulting grain boundary stress state statistics are strongly non-Gaussian. Significant structural evolution is observed within the compressive hold before unloading into tension in the stress profile. Strong angular dependence of grain boundary traction magnitude with shock direction is observed. Non-Schmid effects continue to suggest their influence on propensity of microstructural defect types to nucleate voids. A general void nucleation criterion is proposed using probability theory. The general framework is specified to polycrystalline BCC tantalum in the weak shock regime to include the SVE calculations and literature molecular dynamics calculations of grain boundary void nucleation strength. Probability density functions (PDFs) are used to describe the interaction between the local stress state heterogeneity and the distributed grain boundary void nucleation strength state. A causation entropy maximization procedure removes the requirement for ad hoc selection of a PDF functional form and provides a rigorous procedure for data-based PDF determination. The resulting physically informed PDF describes the spatial appearance frequency of nucleated voids as a function of applied macroscale pressure. Lower length scale physics are thus packaged in a precise and computationally efficient way to provide computational plasticity insight to macroscale dynamic ductile damage models.

36 MATERIALS SCIENCE

Advanced multi-modal mass spectrometry imaging reveals functional differences of placental villous compartments at microscale resolution

The placenta is a complex and heterogeneous organ that links the mother and fetus, playing a crucial role in nourishing and protecting the fetus throughout pregnancy. Integrative spatial multi-omics approaches can provide a systems-level understanding of molecular changes underlying the mechanisms leading to the histological variations of the placenta during healthy pregnancy and pregnancy complications. Herein, we advance our metabolome-informed proteome imaging (MIPI) workflow to include lipidomic imaging, while also expanding the molecular coverage of metabolomic imaging by incorporating on-tissue chemical derivatization (OTCD). The improved MIPI workflow advances biomedical investigations by leveraging state-of-the-art molecular imaging technologies. Lipidome imaging identifies molecular differences between two morphologically distinct compartments of a placental villous functional unit, syncytiotrophoblast (STB) and villous core. Next, our advanced metabolome imaging maps villous functional units with enriched metabolomic activities related to steroid and lipid metabolism, outlining distinct molecular distributions across morphologically different villous compartments. Complementary proteome imaging on these villous functional units reveals a plethora of fatty acid- and steroid-related enzymes uniquely distributed in STB and villous core compartments. Integration across our advanced MIPI imaging modalities enables the reconstruction of active biological pathways of molecular synthesis and maternal-fetal signaling across morphologically distinct placental villous compartments with micrometer-scale resolution.

60 APPLIED LIFE SCIENCES

Development of High Energy Resolution Fluorescence Detection Methods for Advanced Microscale X-ray Absorption Fine Structure Analysis of Critical Elements (Final Report)

This project is developing High-Energy Resolution Fluorescence Detection (HERFD) X-ray Absorption Fine-Structure Spectroscopy (XAFS) at the hard X-ray microprobe beamline at GSECARS beamline 13-ID-E, at the Advanced Photon Source at Argonne National Laboratory. This enhancement will improve sensitivity and spectral interpretation limitations of conventional XAFS which uses energy dispersive solid-state detectors (SSD) to measure the total fluorescence yield (TFY-XAFS). By using high-quality Si and Ge crystal analyzers to select X-ray fluorescence (XRF) from specific emission lines, background signals from other elements or X-ray scattering that can paralyze SSDs can be nearly eliminated, improving the sensitivity to the oxidation and chemical state of dilute species even though the solid angle of the analyzers is relatively small. Furthermore, by using analyzers of low-strain Si or Ge, the energy selection can be smaller than the natural widths of the core electron level. We are particularly interested in applying these enhanced sensitivities to Lanthanide series of rare-earth elements, which are typically at concentrations at or below 10 ppm, and where spectral overlaps with the 3rd row transition metals degrade sensitivity.

47 OTHER INSTRUMENTATION