Search NASA⌕ Search

SEARCH · Search NASA

Results for “Optical microscopy”

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.

Quote a phrase for an exact phrase match. Source license links do not imply unrestricted reuse.

At least 883 records · Page 49
All sourcesNASA NTRSDOE OSTI
DOE OSTI2023

Enhanced lightning strike protection using vertically oriented carbon fiber melded with conventional carbon fiber-reinforced composite and its validation through damage analysis

Lightning strike protection (LSP) is one of the prime factors in aerospace and wind industries concerning safety, enhanced service life, and reduced downtime. To ensure better LSP, high electrical conductivity is required to dissipate the current, which is always a challenge for polymer composites due to the inherent insulating nature of the polymer matrix. Conventional carbon fiber-reinforced composites (CFRP) offer electrical conductivity in the planar direction while the vertical i.e. through-thickness conductivity still remains a challenge. Having been motivated by this fact, we have fabricated CFRP interleaved with vertically oriented CF (Z-fiber) for the lightning strike test (100 kA). A paint was applied to mimic the actual service condition of the composite laminates. We have prepared two Z-fiber composites: (a) Z-1 containing one Z-fiber layer on the top along with conventional CF layers and (b) Z-5 containing five interleaved Z-fiber layers and compared the properties with conventional CFRP (Z-0). Interestingly, even a single Z-fiber layer (Z-1) showed lower damage (visual damage diameter 22 mm) than Z-0 (visual damage diameter 26 mm). Z-5 displayed the lowest damage (visual damage diameter 16.7 mm), which was further confirmed by cross-sectional optical microscopy. Improved LSP was attributed to the higher through-thickness electrical conductivity in the case of Z-5 (9 times with respect to Z-0) reflecting a lower electrical anisotropy for Z-fiber composites. The residual mechanical property after the lightning test was analyzed through the flexural test, and the retention of flexural strength and modulus was 66% and 86%, respectively for Z-5 showing a significant improvement in comparison to Z-0 (>40% for both).

Saha, Subhabrata↗
DOE OSTI2013

Infrared near-field spectroscopy of trace explosives using an external cavity quantum cascade laser

Utilizing a broadly-tunable external cavity quantum cascade laser for scattering-type scanning near-field optical microscopy (s-SNOM), we measure infrared spectra of explosives particles by probing characteristic nitro-group resonances in the 7.1-7.9 µm wavelength range. Measurements are presented with spectral resolution of 0.25 cm-1, spatial resolution of 25 nm, <100 attomolar sensitivity, and at a rapid acquisition time of 90 s per spectrum. We demonstrate high reproducibility of the acquired s-SNOM spectra with very high signal-to-noise ratios and relative noise of <0.02 in self-homodyne detection.

(140.5965) Semiconductor lasers, quantum cascade↗
DOE OSTI2015

Broadband infrared vibrational nano-spectroscopy using thermal blackbody radiation

Infrared vibrational nano-spectroscopy based on scattering scanning near-field optical microscopy (s-SNOM) provides intrinsic chemical specificity with nanometer spatial resolution. Here we use incoherent infrared radiation from a 1400 K thermal blackbody emitter for broadband infrared (IR) nano-spectroscopy.With optimized interferometric heterodyne signal amplification we achieve few-monolayer sensitivity in phonon polariton spectroscopy and attomolar molecular vibrational spectroscopy. Near-field localization and nanoscale spatial resolution is demonstrated in imaging flakes of hexagonal boron nitride (hBN) and determination of its phonon polariton dispersion relation. The signal-to-noise ratio calculations and analysis for different samples and illumination sources provide a reference for irradiance requirements and the attainable near-field signal levels in s-SNOM in general. As a result, the use of a thermal emitter as an IR source thus opens s-SNOM for routine chemical FTIR nano-spectroscopy.

36 MATERIALS SCIENCE↗
DOE OSTI2017

The role of defects in laser-induced modifications of silica coatings and fused silica using picosecond pulses at 1053 nm: I Damage morphology

Laser-induced damage with ps pulse widths straddles the transition from intrinsic, multi-photon ionization and avalanche ionization-based ablation with fs pulses to defect-dominated, thermal-based damage with ns pulses. We investigated the morphology of damage for fused silica and silica coatings between 1 ps and 60 ps at 1053 nm. Using calibrated laser-induced damage experiments, in situ imaging, and high-resolution optical microscopy, atomic force microscopy, and scanning electron microscopy, we show that defects play an important role in laser-induced damage down to 1 ps. Three types of damage are observed: ablation craters, ultra-high density pits, and smooth, circular depressions with central pits. For 10 ps and longer, the smooth, circular depressions limit the damage performance of fused silica and silica coatings. The observed high-density pits and material removal down to 3 ps indicate that variations in surface properties limit the laser-induced damage onset to a greater extent than expected below 60 ps. Below 3 ps, damage craters are smoother although there is still evidence as seen by AFM of inhomogeneous laser-induced damage response very near the damage onset. These results show that modeling the damage onset only as a function of pulse width does not capture the convoluted processes leading to laser induced damage with ps pulses. It is necessary to account for the effects of defects on the processes leading to laser-induced damage. In conclusion, the effects of isolated defects or inhomogeneities are most pronounced above 3 ps but are still discernible and possibly important down to the shortest pulse width investigated here.

42 ENGINEERING↗
DOE OSTI2015

Radiation damage by light- and heavy-ion bombardment of single-crystal LiNbO₃

In this work, a battery of analytical methods including in situ RBS/C, confocal micro-Raman, TEM/STEM, EDS, AFM, and optical microscopy were used to provide a comparative investigation of light- and heavy-ion radiation damage in single-crystal LiNbO₃. High (~MeV) and low (~100s keV) ion energies, corresponding to different stopping power mechanisms, were used and their associated damage events were observed. In addition, sequential irradiation of both ion species was also performed and their cumulative depth-dependent damage was determined. It was found that the contribution from electronic stopping by high-energy heavy ions gave rise to a lower critical fluence for damage formation than for the case of low-energy irradiation. Such energy-dependent critical fluence of heavy-ion irradiation is two to three orders of magnitude smaller than that for the case of light-ion damage. In addition, materials amorphization and collision cascades were seen for heavy-ion irradiation, while for light ion, crystallinity remained at the highest fluence used in the experiment. The irradiation-induced damage is characterized by the formation of defect clusters, elastic strain, surface deformation, as well as change in elemental composition. In particular, the presence of nanometric-scale damage pockets results in increased RBS/C backscattered signal and the appearance of normally forbidden Raman phonon modes. The location of the highest density of damage is in good agreement with SRIM calculations. (author)

36 MATERIALS SCIENCE↗
DOE OSTI2017

The in vivo structure of biological membranes and evidence for lipid domains

Examining the fundamental structure and processes of living cells at the nanoscale poses a unique analytical challenge, as cells are dynamic, chemically diverse, and fragile. A case in point is the cell membrane, which is too small to be seen directly with optical microscopy and provides little observational contrast for other methods. As a consequence, nanoscale characterization of the membrane has been performed ex vivo or in the presence of exogenous labels used to enhance contrast and impart specificity. Here, we introduce an isotopic labeling strategy in the gram-positive bacterium Bacillus subtilis to investigate the nanoscale structure and organization of its plasma membrane in vivo. Through genetic and chemical manipulation of the organism, we labeled the cell and its membrane independently with specific amounts of hydrogen (H) and deuterium (D). These isotopes have different neutron scattering properties without altering the chemical composition of the cells. From neutron scattering spectra, we confirmed that the B. subtilis cell membrane is lamellar and determined that its average hydrophobic thickness is 24.3 ± 0.9 Ångstroms (Å). Furthermore, by creating neutron contrast within the plane of the membrane using a mixture of H- and D-fatty acids, we detected lateral features smaller than 40 nm that are consistent with the notion of lipid rafts. These experiments—performed under biologically relevant conditions—answer long-standing questions in membrane biology and illustrate a fundamentally new approach for systematic in vivo investigations of cell membrane structure.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2022

Dynamically tunable second-harmonic generation using hybrid nanostructures incorporating phase-change chalcogenides

Nonlinear metasurfaces with high conversion efficiencies have been vastly investigated. However, strong dynamic tunability of such devices is limited in conventional passive plasmonic and dielectric material platforms. Germanium antimony telluride (GST) is a promising phase-change chalcogenide for the reconfiguration of metamaterials due to strong nonvolatile changes of the real and imaginary parts of the refraction index through amorphous-crystalline phase change. The orderly structured GST has an even higher potential in tunable second-harmonic generation (SHG) with a non-centrosymmetric crystal structure at the crystalline phase, while the amorphous phase of GST does not exhibit bulk second-order nonlinearity. Here, we experimentally demonstrate SHG switches by actively controlling the crystalline phase of GST for a GST-based hybrid metasurface featuring a gap-surface plasmon resonance, and a quarter-wave asymmetric Fabry–Perot (F–P) cavity incorporating GST. We obtain SHG switches with modulation depths as high as ~ 20 dB for the wavelengths at the on-state resonance. We also demonstrate the feasibility of multi-level SHG modulation by leveraging three controlled GST phases, i.e., amorphous, semi-crystalline, and crystalline, for the gap-surface plasmon hybrid device, which features stronger light–matter interaction and has higher resonant SHG efficiencies than the asymmetric F–P cavity device at respective GST phases. This research reveals that GST-based dynamic SHG switches can be potentially employed in practical applications, such as microscopy, optical communication, and photonic computing in the nonlinear regime.

42 ENGINEERING↗
DOE OSTI2012

Three-Dimensional Imaging and Quantification of Biomass and Biofilms in Porous Media

A new method to resolve biofilms in three dimensions in porous media using high-resolution synchrotron-based x-ray computed microtomography (CMT) has been developed. Imaging biofilms in porous media without disturbing the natural spatial arrangement of the porous media and associated biofilm has been a challenging task, primarily because porous media generally precludes conventional imaging via optical microscopy; x-ray tomography offers a potential alternative. One challenge for using this method is that most conventional x-ray contrast agents are water-soluble and easily diffuse into biofilms. To overcome this problem, silver-coated microspheres were added to the fluid phase to create an x-ray contrast that does not diffuse into the biofilm mass. Using this approach, biofilm imaging in porous media was accomplished with sufficient contrast to differentiate between the biomass- and fluid-filled pore spaces. The method was validated by using a two-dimensional micro-model flow cell where both light microscopy and CMT imaging were used to im age the biofilm. The results of this work has been published in Water Resources Research (Iltis et al., 2010). Additional work needs to be done to optimize this imaging approach, specifically, we find that the quality of the images are highly dependent on the coverage of the biofilm with Ag particles, - which means that we may have issues in dead-end pore space and for very low density (fluffy) biofilms. What we can image for certain with this technique is the biofilm surface that is well-connected to flow paths and thus well-supplied with nutrients etc.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2012

Improved LWR Cladding Performance by EPD Surface Modification Technique

This project will utilize the electro-phoretic deposition technique (EPD) in conjunction with nanofluids to deposit oxide coatings on prototypic zirconium alloy cladding surfaces. After demonstrating that this surface modification is reproducible and robust, the team will subject the modified surface to boiling and corrosion tests to characterize the improved nucleate boiling behavior and superior corrosion performance. The scope of work consists of the following three tasks: The first task will employ the EPD surface modification technique to coat the surface of a prototypic set of zirconium alloy cladding tube materials (e.g. Zircaloy and advanced alloys such as M5) with a micron-thick layer of zirconium oxide nanoparticles. The team will characterize the modified surface for uniformity using optical microscopy and scanning-electron microscopy, and for robustness using standard hardness measurements. After zirconium alloy cladding samples have been prepared and characterized using the EPD technique, the team will begin a set of boiling experiments to measure the heat transfer coefficient and critical heat flux (CHF) limit for each prepared sample and its control sample. This work will provide a relative comparison of the heat transfer performance for each alloy and the surface modification technique employed. As the boiling heat transfer experiments begin, the team will also begin corrosion tests for these zirconium alloy samples using a water corrosion test loop that can mimic light water reactor (LWR) operational environments. They will perform extended corrosion tests on the surface-modified zirconium alloy samples and control samples to examine the robustness of the modified surface, as well as the effect on surface oxidation

22 GENERAL STUDIES OF NUCLEAR REACTORS↗
DOE OSTI2013

Improving 6061-Al Grain Growth and Penetration across HIP-Bonded Clad Interfaces in Monolithic Fuel Plates: Initial Studies

Grain penetration across aluminum-aluminum cladding interfaces in research reactor fuel plates is desirable and was obtained by a legacy roll-bonding process, which attained 20-80% grain penetration. Significant grain penetration in monolithic fuel plates produced by Hot Isostatic Press (HIP) fabrication processing is equally desirable but has yet to be attained. The goal of this study was to modify the 6061-Al in such a way as to promote a much greater extent of crossinterface grain penetration in monolithic fuel plates fabricated by the HIP process. This study documents the outcomes of several strategies attempted to attain this goal. The grain response was characterized using light optical microscopy (LOM) electron backscatter diffraction (EBSD) as a function of these prospective process modifications done to the aluminum prior to the HIP cycle. The strategies included (1) adding macroscopic gaps in the sandwiches to enhance Al flow, (2) adding engineering asperities to enhance Al flow, (3) adding stored energy (cold work), and (4) alternative cleaning and coating. Additionally, two aqueous cleaning methods were compared as baseline control conditions. The results of the preliminary scoping studies in all the categories are presented. In general, none of these approaches were able to obtain >10% grain penetration. Recommended future work includes further development of macroscopic grooving, transferred-arc cleaning, and combinations of these with one another and with other processes.

36 MATERIALS SCIENCE↗
DOE OSTI2013

Energy-Saving Melting and Revert Reduction Technology (E-SMARRT), Task 5.3: Casting Porosity-Free Grain Refined Magnesium Alloys

The objective of this project was to identify the root causes for micro-porosity in magnesium alloy castings and recommend remedies that can be implemented in production. Three casting magnesium alloys were used to determine the causes of porosity that is a common problem in the magnesium casting industry. These alloys were AM50A, AM60A, and AZ91D, and all were grain refined with C 2 Cl 6 . Gas porosity was found to have little effect if proper degassing methods and foundry practices were used. It was found that sound gating practice, directional solidification towards the riser and generous risering should always dominate in order to produce sound castings. In sand cast magnesium, thermal gradients were found to be an important indicator of heat transfer in the mold. A minimum thermal gradient was found for each alloy that would produce sound castings. There were 2.02°C/cm for AM50A, 1.99°C/cm for AM60A, and 1.97°C/cm for AZ91D. If these gradients are met or exceeded when an area of the casting reaches 50°C below the liquidus for the alloy, the casting will be free of shrinkage porosity in that area. The cooling rates measured during casting magnesium alloys in a pre-heated step permanent mold ranged from 12°F/min in the three inches thick step to 200o F/min in the one inch step. The effect of the cooling rate on the grain size and the mechanical properties was noticeable but not substantial. Grain refining with C 2 Cl 6 had a marked effect on the grain size of the permanent mold step casting. It reduced it by 10-15% in AM50A and by a factor of six in AZ91E from 300 µm to around 55 µm. The mechanical properties of both permanent mold cast AZ91E and AM50A were improved by grain refinement. The most prominent increase was in the elongation of AM50A that more than doubled from 8% to 17%. Computer simulation of porosity was conducted for a well gated commercial wheel casting. The simulation did not predict significant porosity in the wheel. The mechanical testing of tensile specimens excised from the wheel indeed confirmed good properties, in line with the specifications for this alloy. Evidence of minimal micro-porosity was detected in sections cut from the wheel and investigated under optical microscopy. This finding confirms the key role played by utilizing optimal gating and risering practices in minimizing porosity in magnesium castings.

32 ENERGY CONSERVATION, CONSUMPTION, AND UTILIZATI↗
DOE OSTI2013

Global Threat Reduction Initiative Fuel Thermo-Physical Characterization Project: Sample Management Plan

This sample management plan provides guidelines for sectioning, preparation, acceptance criteria, analytical path, and end-of-life disposal for the fuel element segments utilized in the Global Threat Reduction Initiative (GTRI), Fuel Thermo-Physical Characterization Project. The Fuel Thermo-Physical Characterization Project is tasked with analysis of irradiated Low Enriched Uranium (LEU) Molybdenum (U-Mo) fuel element samples to support the GTRI conversion program. Sample analysis may include optical microscopy (OM), scanning electron microscopy (SEM) fuel-surface interface analysis, gas pycnometry (density) measurements, laser flash analysis (LFA), differential scanning calorimetry (DSC), thermogravimetry and differential thermal analysis with mass spectroscopy (TG /DTA-MS), Inductively Coupled Plasma Spectrophotometry (ICP), alpha spectroscopy, and Thermal Ionization Mass Spectroscopy (TIMS). The project will utilize existing Radiochemical Processing Laboratory (RPL) operating, technical, and administrative procedures for sample receipt, processing, and analyses. Test instructions (TIs), which are documents used to provide specific details regarding the implementation of an existing RPL approved technical or operational procedure, will also be used to communicate to staff project specific parameters requested by the Principal Investigator (PI). TIs will be developed, reviewed, and issued in accordance with the latest revision of the RPL-PLN-700, RPL Operations Plan. Additionally, the PI must approve all project test instructions and red-line changes to test instructions.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗
DOE OSTI2014

Development of an Innovative High-Thermal Conductivity UO2 Ceramic Composites Fuel Pellets with Carbon Nano-Tubes Using Spark Plasma Sintering

Uranium dioxide (UO2) is the most common fuel material in commercial nuclear power reactors. Despite its numerous advantages such as high melting point, good high-temperature stability, good chemical compatibility with cladding and coolant, and resistance to radiation, it suffers from low thermal conductivity that can result in large temperature gradients within the UO2 fuel pellet, causing it to crack and release fission gases. Thermal swelling of the pellets also limits the lifetime of UO2 fuel in the reactor. To mitigate these problems, we propose to develop novel UO2 fuel with uniformly distributed carbon nanotubes (CNTs) that can provide high-conductivity thermal pathways and can eliminate fuel cracking and fission gas release due to high temperatures. CNTs have been investigated extensively for the past decade to explore their unique physical properties and many potential applications. CNTs have high thermal conductivity (6600 W/mK for an individual single- walled CNT and >3000 W/mK for an individual multi-walled CNT) and high temperature stability up to 2800°C in vacuum and about 750°C in air. These properties make them attractive candidates in preparing nano-composites with new functional properties. The objective of the proposed research is to develop high thermal conductivity of UO2–CNT composites without affecting the neutronic property of UO2 significantly. The concept of this goal is to utilize a rapid sintering method (5–15 min) called spark plasma sintering (SPS) in which a mixture of CNTs and UO2 powder are used to make composites with different volume fractions of CNTs. Incorporation of these nanoscale materials plays a fundamentally critical role in controlling the performance and stability of UO2 fuel. We will use a novel in situ growth process to grow CNTs on UO2 particles for rapid sintering and develop UO2-CNT composites. This method is expected to provide a uniform distribution of CNTs at various volume fractions so that a high thermally conductive UO2-CNT composite is obtained with a minimal volume fraction of CNTs. The mixtures are sintered in the SPS facility at a range of temperatures, pressures, and time durations so as to identify the optimal processing conditions to obtain the desired microstructure of sintered UO2-CNT pellets. The second objective of the proposed work is to identify the optimal volume fraction of CNTs in the microstructure of the composites that provides the desired high thermal conductivity yet retaining the mechanical strength required for efficient function as a reactor fuel. We will systematically study the resulting microstructure (grain size, porosity, distribution of CNTs, etc.) obtained at various SPS processing conditions using optical microscopy, scanning electron microscopy (SEM), and transmission electron microscope (TEM). We will conduct indentation hardness measurements and uniaxial strength measurements as a function of volume fraction of CNTs to determine the mechanical strength and compare them to the properties of UO2. The fracture surfaces will be studied to determine the fracture characteristics that may relate to the observed cracking during service. Finally, we will perform thermal conductivity measurements on all the composites up to 1000° C. This study will relate the microstructure, mechanical properties, and thermal properties at various volume fractions of CNTs. The overall intent is to identify optimal processing conditions that will provide a well-consolidated compact with optimal microstructure and thermo-mechanical properties. The deliverables include: (1) fully characterized UO2-CNT composite with optimal CNT volume fraction and high thermal conductivity and (2) processing conditions for production of UO2-CNT composite pellets using SPS method.

Subhash, Ghatu↗
DOE OSTI2014

Exploring Charge Transport in Guest Molecule Infiltrated Cu 3 (BTC) 2 Metal Organic Framework

The goal of this Exploratory Express project was to expand the understanding of the physical properties of our recently discovered class of materials consisting of metal-organic frameworks with electroactive ‘guest’ molecules that together form an electrically conducting charge-transfer complex (molecule@MOF). Thin films of Cu 3 (BTC) 2 were grown on fused silica using solution step-by-step growth and were infiltrated with the molecule tetracyanoquinodimethane (TCNQ). The infiltrated MOF films were extensively characterized using optical microscopy, scanning electron microscopy, Raman spectroscopy, electrical conductivity, and thermoelectric properties. Thermopower measurements on TCNQ@Cu 3 (BTC) 2 revealed a positive Seebeck coefficient of ~400 μV/k, indicating that holes are the primary carriers in this material. The high value of the Seebeck coefficient and the expected low thermal conductivity suggest that molecule@MOF materials may be attractive for thermoelectric power conversion applications requiring low cost, solution-processable, and non-toxic active materials.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2014

Advanced Test Reactor National Scientific User Facility (ATR NSUF) (Monthly Report, December 2014)

PNNL has completed sectioning of the U.C. Berkeley hydride fuel rodlet 1 (highest burn-up) and is currently polishing samples in preparation for optical metallography. A disk was successfully sectioned from rodlet 1 at the location of the internal thermocouple tip as desired. The transition from annular pellet to solid pellet is verified by the eutectic-filled inner cavity located on the back face of this disk (top left) and the solid front face (bottom left). Preliminary low-resolution images indicate interesting sample characteristics in the eutectic surrounding the rodlet at the location of the outer thermocouple tip (right). This sample has been potted and is currently being polished for high-resolution optical microscopy and subsequent SEM analysis.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2015

Complete Initial Scoping Tests on the Incorporation of Novel Loaded Iodine Getters into GCM

This study encompasses initial scoping tests on the incorporation of a novel iodine loaded getter material into the Sandia developed low temperature sintering glass ceramic material (GCM) waste form. In particular, we studied the PNNL Ag-I-Aerogel. Optical microscopy indicates inhomogenous samples based on particle sizes and variations in color (AgI vs Ag/AgO on silica). TGA/MS data when heated in air indicates loss of iodine and organics (CO2) between 250-450°C a total of ~15wt% loss, with additional / small iodine loss when during 550°C hold for 1 hr. TGA/MS data when heated in N2 indicates less organic and slightly less iodine loss below 550°C, with no loss of iodine in 550°C 1 hour hold. Furthermore, a substantial mass loss of sulfur containing compounds is observed (m/e of 34 and 36) between 150 – 550°C in both air and N2 sintering atmospheres. In an effort to capture iodine lost to volatilization during heating (at temps below glass sintering temperature of 550°C), we added 5 wt% Ag flake to the AgIaerogel. Resulting data indicates the iodine is retained with the addition of the Ag flake, resulting in only a small iodine loss (< 1wt%) at ~350°C. No method of curtailing loss of sulfur containing compounds due to heating was successful in this scoping study.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2015

Demonstration of thermal control, microstructure control, defect mitigation and process parameter database generation for Ti-6Al-4V Direct Digital Manufacturing - Understanding defect mitigation and process parameter database generation for direct digital manufacturing

Researchers from Manufacturing Demonstration Facility (MDF) at Oak Ridge National Laboratory (ORNL) worked with Applied Optimization (AO) to understand and evaluate the propensity for defect formation in builds manufactured using DM3D-POM laser direct metal deposition. The main aim of this collaboration was to understand the character of powder jet behavior as a function of the nozzle parameters such as cover gas, carrier gas, and shaping gas. In order to evaluate the sensitivities of the parameters used in model, various experiments were performed with in-situ monitoring of the powder stream characteristics using a high speed camera. A wide variety of conditions while keeping the hopper motor rpm constant, including laser power and travel speed were explored. The cross sections of the deposits were characterized using optical microscopy.

47 OTHER INSTRUMENTATION↗
DOE OSTI2012

Freezing in porous media: Phase behavior, dynamics and transport phenomena

This research was focused on developing the underlying framework for the mechanisms that control the nature of the solidification of a broad range of porous media. To encompass the scope of porous media under consideration we considered material ranging from a dilute colloidal suspension to a highly packed saturated host matrix with a known geometry. The basic physical processes that occur when the interstitial liquid phase solidifies revealed a host of surprises with a broad range of implications from geophysics to materials science and engineering. We now understand that ostensibly microscopic films of unfrozen liquid control both the equilibrium and transport properties of a highly packed saturated host matrix as well as a rather dilute colloidal suspension. However, our description of the effective medium behavior in these settings is rather different and this sets the stage for the future research based on our past results. Once the liquid phase of a saturated relatively densely packed material is frozen, there is a rich dynamical behavior of particles for example due to the directed motion driven by thermomolecular pressure gradients or the confined Brownian motion of the particles. In quite striking contrast, when one freezes a dilute suspension the behavior can be rather more like that of a binary alloy with the particles playing the role of a ``solute''. We probed such systems quantitatively by (i) using X ray photon correlation spectroscopy (XPCS) and Small Angle X-ray Scattering (SAXS) at the Advanced Photon Source at Argonne (ii) studying the Argonne cell in the laboratory using optical microscopy and imagery (because it is not directly visible while in the vacuum can). (3) analyzed the general transport phenomena within the framework of both irreversible thermodynamics and alloy solidification and (4) applied the results to the study of the redistribution of solid particles in a frozen interstitial material. This research has gone a long way towards establishing a quantitative foundation for a wide class of problems in environmental and technological settings.

54 ENVIRONMENTAL SCIENCES↗