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NASA NTRS2002

Infrared Spectroscopy as a Chemical Fingerprinting Tool

Infrared (IR) spectroscopy is a powerful analytical tool in the chemical fingerprinting of materials. The technique is rapid, reproducible and usually non-invasive. With the appropriate accessories, the technique can be used to examine samples in either a solid, liquid or gas phase. Solid samples of varying sizes and shapes may be used, and with the addition of microscopic IR (microspectroscopy) capabilities, minute materials such as single fibers and threads may be examined. With the addition of appropriate software, microspectroscopy can be used for automated discrete point or compositional surface area mapping, with the latter providing a means to record changes in the chemical composition of a material surface over a defined area. Both aqueous and non-aqueous free-flowing solutions can be analyzed using appropriate IR techniques, as can viscous liquids such as heavy oils and greases. Due to the ability to characterize gaseous samples, IR spectroscopy can also be coupled with thermal processes such as thermogravimetric (TG) analyses to provide both thermal and chemical data in a single run. In this configuration, solids (or liquids) heated in a TG analyzer undergo decomposition, with the evolving gases directed into the IR spectrometer. Thus, information is provided on the thermal properties of a material and the order in which its chemical constituents are broken down during incremental heating. Specific examples of these varied applications will be cited, with data interpretation and method limitations further discussed.

Huff, Tim↗

DOE OSTI2025

Multiphase Processing of the Water-Soluble and Insoluble Phases of Biomass Burning Organic Aerosol

Biomass burning is one of the most significant sources of organic aerosol in the atmosphere. Biomass burning organic aerosol (BBOA) has been observed to undergo liquid– liquid phase separation (LLPS) to give core–shell morphology with the hydrophobic phase encapsulating the hydrophilic phase, potentially impacting the evolution of light-absorbing components, i.e., brown carbon (BrC), through multiphase processes. Here, we demonstrate how multiphase processing differs between the watersoluble (i.e., hydrophilic) and insoluble (i.e., hydrophobic) phases of BBOA in terms of reactive uptake of ozone in a coated-wall flow tube. Effects of relative humidity (RH) and ultraviolet (UV) irradiation were investigated. Experimental timeseries were used to inform simulations using multilayer kinetic modeling. Among non-irradiated thin films, the uptake coefficient was greatest for the water-soluble phase at 75% RH (3 × 10 –5 , corresponding to a diffusion coefficient of BrC, D BrC , of 3 × 10 –9 cm 2 s –1 ) and least for the same phase at 0% RH (1 × 10 –5 , corresponding to D BrC of 1 × 10 –10 cm 2 s –1 ). The uptake coefficient for the water-insoluble phase fell between these two (about 1.5 × 10 –5 ), regardless of RH, and the corresponding D BrC increased only slightly (8 × 10 –10 cm 2 s –1 at 0% RH to 9 × 10 –10 cm 2 s –1 at 75% RH). The uptake coefficients of both phases at 0% RH decreased significantly after UV irradiation, consistent with a transition from viscous liquid to solid and supported by qualitative microscopy observations. Modeling multiphase ozone oxidation of primary BrC components in the atmosphere demonstrated, first, that LLPS may extend the lifetime of water-soluble BBOA encapsulated by water-insoluble species by a factor of 1.5 at moderate to high RH and, also, that UV irradiation may extend the lifetime of both phases by more than a factor of 2.5.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2025

Chemically Recyclable Polyester Thermosets from Activated Adipic Acid and Renewable Polyols

This study outlines a method for producing chemically recyclable crosslinked polyesters using renewable polyols-glycerol and sorbitol-combined with adipic acid (AA), which is transformed/activated into a polyanhydride mixture prior to use. A three-step procedure has been designed: 1) an acid-catalyzed reaction of AA with nontoxic isopropenyl acetate or acetic anhydride to form a crosslinking mixture (CLM) made of adipic-acetic mixed polyanhydrides; 2) a solvent- and additive-free process where glycerol or sorbitol, or a combination thereof, is reacted with the CLM to achieve a prepolymer, and 3) a casting/molding of the liquid viscous prepolymer to yield a thermoset as the end product. Different thermosets (eight examples) are prepared by changing the reagents ratio. These solids are thoroughly characterized by tensile tests, DMA, high-resolution magic angle spinning and solid-state NMR, thermal gravimetric analysis, DSC, and fourier transformed infra red (FT-IR) spectroscopy. The formation of cross-linked polyesters is confirmed in all cases, but mechanical properties varied significantly from one specimen to another. Interestingly, a tensile strength up to 18 MPa-approximately an order of magnitude higher than similar polymers-is achieved when sorbitol and the CLM are used in a 1:1 wt% ratio. The chemical recycle of the resulting polymers is achieved via methanolysis with quantitative recovery of the monomeric units.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2021

When SLIPS meets TIPS: An endogenous lubricant-infused surface by taking the diluent as the lubricant

Slippery lubricant-infused porous surfaces (SLIPSs) hold great promise in fields requiring adhesion resistance such as self-cleaning, anti-fouling, anti-icing, and anti-scaling. However, their road to practical application is still blocked by the complicated fabrication process and the restricted coating area. To address these challenges, we propose a new concept of endogenous SLIPS in which the porous structure grows from the solution coating of polypropylene/caprylyl methicone undergoing a thermally induced phase separation (TIPS) process. Caprylyl methicone serves as the diluent during TIPS as well as the lubricant in the SLIPS so that the coating can be fabricated in one step and unrestrictedly. Furthermore, the dissolution and phase separation mechanisms have been revealed by molecular dynamic simulation and in situ microscopic observation. Such SLIPSs exhibits impressive sliding property even for sticky and viscous liquids and exhibit extremely low ice adhesion in anti-icing tests.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2022

Odd-viscosity-induced passivation of Moffatt vortices

Odd viscosity is associated with a number of striking physical phenomena: a disk rotating in a viscous liquid experiences a normal compressive or tensile stress depending on its sense of rotation; chiral active matter interfacial deformations level off in a manner akin to surface tension; and unstable thermocapillary films become stabilized. In this article we show that odd viscosity decreases the size and intensity of Moffatt vortices in a corner formed by a solid substrate and a free interface. The effect is present because odd viscosity creates a normal-stress-induced shear stress at the liquid–gas interface. The new shear stress is out of phase and oppositely directed with respect to the interfacial liquid velocity. It squeezes the vortices and damps their rotation. As a consequence, Moffatt vortices can now be observed with greater facility in an experiment. Odd viscosity also increases the range of corner angles over which Moffatt vortices can be observed, and, in general, it shows a tendency to moderate singular behaviour.

Mechanics↗

NASA NTRS1964

Viscous-pendulum damper suppresses structural vibrations

The viscous pendulum damper consists of a cylinder containing round trays on which round lead slugs rest. When assembled, the container is filled with a viscous liquid and attached, with axis vertical, to the structure. The device permits varying the damping of structural vibrations.

Reed, W. H., III↗

NASA NTRS1973

Extended hydrodynamic theory of the peak and minimum pool boiling heat fluxes

The hydrodynamic theory of the extreme pool boiling heat fluxes is expanded to embrace a variety of problems that have not previously been analyzed. These problems include the prediction of the peak heat flux on a variety of finite heaters, the influence of viscosity on the Taylor and Helmoltz instability mechanisms with application to film boiling and to the peak heat flux in viscous liquids, the formalization of the analogy between high-current-density electrolysis and boiling, and the description of boiling in the low-gravity limit. The predictions are verified with a large number of new data.

Linehard, J. H.↗

NASA NTRS1979

Study of polyphenyl ether fluid /5P4E/ in operating elastohydrodynamic contacts by infrared emission spectroscopy

Infrared emission spectra of 5P4E polyphenyl ether were obtained from an operating elastohydrodynamic sliding contact at different speeds and loads by Fourier emission microspectrophotometry. The spectra were found to be polarized with respect to the direction of the conjunction line, especially at high shear rates. Film and metal surface temperatures were calculated from the spectra, and film thicknesses were determined under various operating conditions. Changes of polarized band structure above a critical shear rate, at which the slope of the film temperature versus shear curve changes abruptly and at which the film thickness assumes a minimum value, are consistent with a transition of the lubricant from a viscous liquid to a viscoelastic liquid or to an elastic solid.

Lauer, J. L.↗

NASA NTRS1980

Convective flows of viscous fluid in spherical layers. Certain astrophysical applications

The convective stability of a viscous liquid in spherical layers is investigated taking into consideration rotation, the latitudinal temperature gradient, and shear flow. The results of calculating nonlinear convective motion in spherical layers are examined. A discussion is given of the applicability of the results obtained to studying convection in astrophysical objects.

Yavorskaya, I. M.↗

NASA NTRS1982

Gas-Jet Levitation Furnace

Gas jet levitates solid and viscous liquid spheroids at high temperatures in new contactless processing system. System can be used to observe high temperature transformations (for example, crystallization without contact with another solid surface) or in containerless studies to eliminate contamination by crucible.

Ethridge, E. C.↗

NASA NTRS1979

Measurement of diffusion coefficients from solution rates of bubbles

The rate of solution of a stationary bubble is limited by the diffusion of dissolved gas molecules away from the bubble surface. Diffusion coefficients computed from measured rates of solution give mean values higher than accepted literature values, with standard errors as high as 10% for a single observation. Better accuracy is achieved with sparingly soluble gases, small bubbles, and highly viscous liquids. Accuracy correlates with the Grashof number, indicating that free convection is the major source of error. Accuracy should, therefore, be greatly increased in a gravity-free environment. The fact that the bubble will need no support is an additional important advantage of Spacelab for this measurement.

Krieger, I. M.↗

NASA NTRS1983

Vortices, stability, and turbulence

The transition process between laminar flow to turbulent flow is discussed in terms of a third state of fluid motion, vortical motion that is approximately periodic in space and/or time and displays symmetrical properties. The possibility that the transition from laminar to turbulent flow is accompanied by intermediate vortical states, with turbulence being an instability of the vortical states, is examined, with consideration given to the hypothesis that the turbulent state retains a memory of the vortex structures. Solutions are sought for the Navier-Stokes equations for a viscous liquid in a channel. Instances of inviscid vortical states and the presence of a three-dimensional instability are studied, demonstrating that transition phenomena can be explained qualitatively in terms of vortical state characteristics.

Saffman, P. G.↗

NASA NTRS1985

Improved Coulomb-Friction Damper

Equal damping provided on forward and reverse strokes. Improved damper has springs and wedge rings symmetrically placed on both ends of piston wedge, so friction force same in both directions of travel. Unlike conventional automotive shock absorbers, they resemble on outside, both versions require no viscous liquid and operate over wide temperature range.

Campbell, G. E.↗

NASA NTRS1985

Shape instability in thin viscous films and jets

The theory of viscous liquid films and thin jets as two- and one-dimensional continua is examined. Theoretical results are presented concerning a special type of instability which leads to the loss of smoothness of the shape (wrinkling) and associated with the failure of hyperbolicity of the governing equations. The conditions for different types of such an instability are formulated in the closed analytical form.

Zak, M.↗

NASA NTRS1985

Undercooling, Remelting, and Coarsening

Solidification of metal alloys with initial high undercoolings occurs with rapid recalescence due to rapid heat release of the latent heat of fusion. The recalescence temperature is usually higher than the solidus and/or the thermodynamic T sub o temperature of the alloy, depending on the initial undercooling and alloy composition. The rapid heating during recalescence alters the initially solidified structures, in ways that must include partial remelting, ripening, coarsening, and decomposition of the rapidly solidified primary metastable or supersaturated phases. New ways to study the solidification and remelting phenomena associated with the rapid heating during recalescence of undercooled alloys were developed. The phenomena are studied by using: (1) emulsions of iron and nickel base alloys in viscous liquid carriers; and (2) rapid heating of metal samples by electric discharge, using a technique similar to the exploding wire process (EWP), except with less power input. Experimental results are combined with theoretical analyses to better understand the solidification of levitated metal droplets with high undercooling, which relates to the solidification process.

Flemings, M. C.↗

NASA NTRS1986

Dynamic dielectric analysis - A means for process control

The development of dynamic dielectric analysis techniques (as a 'smart' sensor for quantitative NDE) and of intelligent closed-loop cure systems is reported. The cure process of both BF3:R-catalyzed and uncatalyzed tetraglycidyl-4,4'-diaminodiphenyl methane (TGDDM)/diamine epoxy resins was studied. Measurements were made over a frequency range of six decades. The resin was monitored continuously throughout the cure process as it changed from a viscous liquid to a highly crosslinked solid. From the frequency dependence of the dielectric loss, the specific conductivity has been determined and shown to directly monitor the viscosity before the gel point is reached. Dielectric master plots of the cure process, analogous to time-temperature superposition plots for rheological data, have been developed.

Kranbuehl, D.↗

NASA NTRS1990

Composite superconducting wires obtained by high-rate tinning in molten Bi-Pb-Sr-Ca-Cu-O system

The preparation of high-T(sub c) superconducting long composite wires by short-time tinning of the metal wires in a molten Bi-Pb-Sr-Ca-Cu-O compound is discussed. The application of this method to the high-T(sub c) materials is tested, possibly for the first time. The initial materials used for this experiment were ceramic samples with nominal composition Bi(1.5)Pb(0.5)Sr2Ca2Cu3O(x) and T(sub c) = 80 K prepared by the ordinary solid-state reaction, and industrial copper wires from 100 to 400 microns in diameter and from 0.5 to 1 m long. The continuously moving wires were let through a small molten zone (approximately 100 cubic mm). The Bi-based high-T(sub c) ceramics in a molten state is a viscous liquid and it has a strongly pronounced ability to spread on metal wire surfaces. The maximum draw rate of the Cu-wire, at which a dense covering is still possible, corresponds to the time of direct contact of wire surfaces and liquid ceramics for less than 0.1 s. A high-rate draw of the wire permits a decrease in the reaction of the oxide melt and Cu-wire. This method of manufacture led to the fabrication of wire with a copper core in a dense covering with uniform thickness of about h approximately equal to 5 to 50 microns. Composite wires with h approximately equal to 10 microns (h/d approximately equal to 0.1) sustained bending on a 15 mm radius frame without cracking during flexing.

Grozav, A. D.↗

NASA NTRS1989

Shear stabilization of the capillary breakup of a cylindrical interface

A cylindrical interface containing a viscous liquid set into axial motion is subject to a capillary and to a surface-wave instability. Clues from previous studies suggest that, even though both mechanisms separately are destabilizing, under certain circumstances their mutual interaction can lead to a stable interface; shear can stabilize capillary breakup. Here, an axial flow through an annular cross section bounded on the inside by a rigid rod and on the outside by a deformable interface is considered. The competition between the two mechanisms is studied through the temporal growth of infinitesimal axisymmetric and nonaxisymmetric disturbances. This examination of temporal stability shows that, indeed, for geometries corresponding to thin annular layers both instabilities can be completely suppressed (disturbances of all wavelengths decay).

Russo, Mathew J.↗