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At least 469 records · Page 26

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NASA NTRS1972

Thermal properties of polymers below 4 K.

Obtained measurement data on the Debye contribution to the specific heat, the specific heat, and the thermal conductivity in polymers below 4 deg K are discussed. The results obtained suggest that impurities are responsible for the apparent thermal properties of polymers and glasses at low temperatures. In order to determine the intrinsic behavior of amorphous solids, measurements must be made at temperatures low enough to freeze out the local modes.

Salinger, G. L.↗

NASA NTRS1976

Holographic Recording Materials Development

Organic photorefractive materials were evaluated for application in a reversible holographic memory system. Representative indigo and thioindigo derivatives and several stilbene derivatives were studied as well as 15, 16-dialkyldihydropyrene derivatives the following goals were achieved: (1) the successful writing of phase holograms in a thioindigo/polymer gel system, (2) the successful writing and erasing of phase holograms in a variety of indigo/polymer gel and indigo/solid polymer systems, and (3) the identification of indigoid dyes and 15, 16-dialkyldihydropyrene derivatives as materials potentially suitable for utilization in an operational system. Photochemical studies of the stilbene, indigo, thioindigo, and dialkyldihydropyrene derivatives in solution and in a variety of polymer matrix materials were conducted with the goal of optimizing the photorefractive behavior of the chemical system as a whole. The spectroscopic properties required of optimal photorefractive materials were identified, and it was shown that both the indigoid dyes and the dialkyldihydropyrenes closely match the required properties.

Verber, C. M.↗

NASA NTRS2001

Physics of Colloids in Space-2 (PCS-2)

The Physics of Colloids-2 (PCS-2) experiment is aimed at investigating the basic physical properties of several types of colloidal suspensions. The three broad classes of colloidal systems of interest are binary colloids, colloid-polymer mixtures, and fractal gels. The objective is to understand their phase behavior as well as the kinetics of the phase transitions in the absence of gravity. The nucleation, growth, and morphology characteristics of the crystals and gels that form would be studied using confocal microscopy. These will be observed directly with excellent time resolution, and therefore extensive information about the different phases and their growth mechanisms will be gained. With the laser tweezers, it will be possible to measure the strength of these structures and to modify them in a controlled way, and the spectrophotometer will provide the possibility to probe their optical properties. We believe that this experiment will provide the basis for future 'colloid engineering' in which complicated structures with novel properties (e.g., photonic crystals) will be grown by controlled self-assembly.

Sankaran, Subramanian↗

NASA NTRS2004

Field Effect Transistor Behavior in Electrospun Polyaniline/Polyethylene Oxide Demonstrated

Novel transistors and logic devices based on nanotechnology concepts are under intense development. The potential for ultra-low-power circuitry makes nanotechnology attractive for applications such as digital electronics and sensors. For NASA applications, nanotechnology offers tremendous opportunities for increased onboard data processing, and thus autonomous decisionmaking ability, and novel sensors that detect and respond to environmental stimuli with little oversight requirements. Polyaniline/polyethylene oxide (PANi/PEO) nanofibers are of interest because they have electrical conductivities that can be changed from insulating to metallic by varying the doping levels and conformations of the polymer chain. At the NASA Glenn Research Center, we have observed field effect transistor (FET) behavior in electrospun PANi/PEO nanofibers doped with camphorsulfonic acid. The nanofibers were deposited onto Au electrodes, which had been prepatterned onto oxidized silicon substrates. The preceding scanning electron image shows the device used in the transistor measurements. Saturation channel currents are observed at surprisingly low source/drain voltages (see the following graph). The hole mobility in the depletion regime is 1.4x10(exp -4)sq cm/V sec, whereas the one-dimensional charge density (at zero gate bias) is calculated to be approximately 1 hole per 50 two-ring repeat units of polyaniline, consistent with the rather high channel conductivity (approx.10(exp -3) S/cm). Reducing or eliminating the PEO content in the fiber is expected to enhance device parameters. Electrospinning is thus proposed as a simple method of fabricating one-dimensional polymer FET's.

Mueller, Carl H.↗

DOE OSTI2024

Evaluation of Common Thermoplastic Polymers in High-Pressure Cycling Hydrogen Under Ambient and Cold Environments as Applicable to the Hydrogen Infrastructure

Thermoplastic polymers are required to perform unfailingly under stringent conditions of changing pressures (35 MPa to 70 MPa) and temperatures (-40°C to +85°C) in storage and fueling operations. Although diffusivity in glassy polymers appear to be an order of magnitude lower than elastomers, polymer microstructural attributes such as degree of crystallinity and presence of polar and non-polar groups on the main chain with and without branching can play a substantial role in influencing their behaviors in hydrogen environments. In the work described here, the effect of high-pressure hydrogen cycling on PEEK, PTFE, PA11, HDPE, POM (and different commercial grades of these polymers) under ambient and cold (-40°C) conditions is addressed. Ex-situ characterization for polymer changes included density measurements for impact of hydrogen retention, hardness changes using nanoindentation, storage modulus and glass transition changes using dynamic mechanical and thermal analysis (DMTA), degree of crystallization with Differential Scanning Calorimetry (DSC) and tensile testing following ASTM D412. In other evaluations, solid-state nuclear magnetic resonance (NMR), attenuated total reflectance Fourier transform infra-red spectroscopy (ATRFTIR), X-ray diffraction (XRD), and X-ray CT results are presented. The overall impact of these evaluations is to establish a technical basis for the behaviors of common thermoplastics in cycling hydrogen environments under ambient and cold temperatures while establishing the relationship between polymer structure-based properties and hydrogen transport effects.

Menon, Nalini C.↗

DOE OSTI2026

Self-Assembly Driven Microlithography via Near-Infrared Light Activation

Current vat photopolymerization (VP) relies on UV or visible light to start the rapid crosslinking of liquid photocurable resins into 3D-printed structures. Here, we develop a self-assembly-driven photopatterning approach to photothermally generate polymeric solids by combining thermoplasmonic nanoparticles and thermoresponsive polymers, in which near-infrared (NIR) light activates thermoplasmonic heating of nanoparticles, triggering the irreversible self-assembly of thermoresponsive polymers into insoluble mesoglobules. A small amount of thermal initiator and crosslinker leads to irreversible self-assembly of polymer nanocomposites. NIR light offers deeper penetration and reduced scattering compared to UV, enabling more uniform curing of thicker or filled materials and expanded process control for composites or opaque systems. Thermoplasmonic heat generation is achieved using surface-modified gold nanorods (AuNRs) with a longitudinal localized surface plasmon resonance peak in the NIR region. Key variables such as polymer composition, molecular weight, physical interactions at the nanoparticle–polymer interface, which can be tuned by surface functionalization, AuNR concentration, and pH can be used to tailor the assembly behavior of these systems, including photothermal effect, flocculation, and cloud point temperature, and the mechanical properties of the final structures. Collectively, these results highlight a platform for photothermally-driven microlithography of polymer solids with diverse, tunable macroscopic properties, enabled by low-energy NIR light-activated self-assembly.

36 MATERIALS SCIENCE↗

NASA NTRS2003

Composite-Based High Performance Electroactive Polymers For Remotely Controlled Mechanical Manipulations in NASA Applications

This program supported investigation of an all-polymer percolative composite which exhibits very high dielectric constant (less than 7,000). The experimental results show that the dielectric behavior of this new class of percolative composites follows the prediction of the percolation theory and the analysis of the conductive percolation phenomena. The very high dielectric constant of the all-polymer composites which are also very flexible and possess elastic modulus not very much different from that of the insulation polymer matrix makes it possible to induce a high electromechanical response under a much reduced electric field (a strain of 2.65% with an elastic energy density of 0.18 J/cu cm can be achieved under a field of 16 MV/m). Data analysis also suggests that in these composites, the non-uniform local field distribution as well as interface effects can significantly enhance the strain responses. Furthermore, the experimental data as well as the data analysis indicate that the conduction loss in these composites will not affect the strain hysteresis.

Zhang, Q. M.↗

NASA NTRS2000

Nonlinearity and Strain-Rate Dependence in the Deformation Response of Polymer Matrix Composites Modeled

There has been no accurate procedure for modeling the high-speed impact of composite materials, but such an analytical capability will be required in designing reliable lightweight engine-containment systems. The majority of the models in use assume a linear elastic material response that does not vary with strain rate. However, for containment systems, polymer matrix composites incorporating ductile polymers are likely to be used. For such a material, the deformation response is likely to be nonlinear and to vary with strain rate. An analytical model has been developed at the NASA Glenn Research Center at Lewis Field that incorporates both of these features. A set of constitutive equations that was originally developed to analyze the viscoplastic deformation of metals (Ramaswamy-Stouffer equations) was modified to simulate the nonlinear, rate-dependent deformation of polymers. Specifically, the effects of hydrostatic stresses on the inelastic response, which can be significant in polymers, were accounted for by a modification of the definition of the effective stress. The constitutive equations were then incorporated into a composite micromechanics model based on the mechanics of materials theory. This theory predicts the deformation response of a composite material from the properties and behavior of the individual constituents. In this manner, the nonlinear, rate-dependent deformation response of a polymer matrix composite can be predicted.

Goldberg, Robert K.↗

NASA NTRS2001

Extensional Rheology Experiment Developed to Investigate the Rheology of Dilute Polymer Solutions in Microgravity

A fundamental characteristic of fluid is viscosity; that is, the fluid resists forces that cause it to flow. This characteristic, or parameter, is used by manufacturers and end-users to describe the physical properties of a specific material so that they know what to expect when a material, such as a polymer, is processed through an extruder, a film blower, or a fiber-spinning apparatus. Normally, researchers will report a shear viscosity that depends on the rate of an imposed shearing flow. Although this type of characterization is sufficient for some processes, simple shearing experiments do not provide a complete picture of what a processor may expect for all materials. Extensional stretching flows are common in many polymer-processing operations such as extrusion, blow molding, and fiber spinning. Therefore, knowledge of the complete rheological (ability to flow and be deformed) properties of the polymeric fluid being processed is required to accurately predict and account for the flow behavior. In addition, if numerical simulations are ever able to serve as a priori design tools for optimizing polymer processing operations such as those described above, an accurate knowledge of the extensional viscosity of a polymer system and its variation with temperature, concentration, molecular weight, and strain rate is critical.

Logsdon, Kirk A.↗

DOE OSTI2025

Sequential Infiltration Synthesis of Multinary Metal Oxides: The Role of Precursor Diffusion and Reactivity

Understanding volatile metal–organic precursor transport in polymer matrices during sequential infiltration synthesis (SIS) is critical to the design of hybrid materials of tailored composition and uniform structure. Here, we investigate the diffusion and reaction behavior of diethylzinc (DEZ) in poly(methyl methacrylate) (PMMA) matrices with variable indium and zinc incorporation. Unlike conventional SIS where precursors adduct or react directly with the polymer backbone, DEZ shows minimal interaction with PMMA. However, DEZ may interact strongly with In–OH or Zn–OH moieties that are previously incorporated into a PMMA thick film. Using spectroscopic ellipsometry, X-ray photoelectron spectroscopy depth profiling, and EDX line scans, we quantify Zn incorporation as a function of exposure time, polymer thickness, and previous infiltration steps. The Zn distribution evolves from surface-localized to deep within the ∼1 μm thick film with increasing DEZ exposures up to 30 min. A reaction-diffusion model incorporating a hindering factor to capture diffusivity decay due to product accumulation reproduces the Zn depth profile and yields physically meaningful parameters to guide future growth. Furthermore, this study provides a framework for interpreting metal–organic precursor infiltration behavior and highlights the utility of model-guided SIS process design.

diethylzinc↗

DOE OSTI2021

Modeling swelling behavior of hydrogels in aqueous organic solvents

Hydrogel, a three-dimensional elastic structure of cross-linked polymer chains, swells or deswells when immersed in aqueous organic solutions. The swelling of hydrogels depends on temperature, solvent composition, and hydrogel structure as the thermodynamic driving forces for hydrogel swelling are due to solvent – hydrogel interactions and expansion of elastic network. Here in this work, polymer Nonrandom Two-Liquid activity coefficient model is used to account for the solvent – hydrogel interactions and a semi-empirical expression for rubber elasticity is used to describe the expansion of elastic network. The model successfully correlates data for both swelling and equilibrium phase compositions for n-isopropyl acrylamide hydrogels in water – ethanol, water – acetone, water – n-butanol, and water – methyl isobutyl ketone mixed solvents.

42 ENGINEERING↗

DOE OSTI2023

Polythiophene-based terpolymers with modulated aggregation behaviors for high-performance organic solar cells with 16.6% efficiency

Polythiophenes (PTs) are an attractive class of polymer donors (PDs) for organic solar cells (OSCs) owing to their relatively simple structures and scalable synthesis. Herein, a series of chlorinated thiazole-incorporated PT terpolymers are designed and high-performance OSCs with a power conversion efficiency (PCE) of 16.6% are demonstrated. By incorporating two different units, 3,3'-difluoro-2,2'-bithiophene (T2F2) and thieno[3,2-b]thiophene (TT), the aggregation properties of the terpolymers (PTz-FX; X = 0, 30, 50, 70, and 100, where X represents the mole percentage of T2F2 to total T2F2 +TT) are modulated. Among the PTz-FX series, PTz-F70 is found to be the optimal P D because its suitably tuned aggregation property leads to an optimized blend morphology with well-developed crystalline structures and donor–acceptor intermixed domains. The balanced morphology not only promotes charge generation/transport but also suppresses charge recombination in OSC devices. Thus, the PTz-F70-based OSCs achieve the highest PCE (16.6%), outperforming the OSCs based on PTz-FX with extremely strong (PTz-F100, PCE = 14.7%) or weak (PTz-F0, PCE = 12.0%) aggregation properties. The PCE of the PTz-F70-based OSCs is one of the highest performances among PT-based binary OSCs. Finally, this study highlights the importance of controlling the aggregation property of PTs for achieving high-performance PT-based OSCs.

14 SOLAR ENERGY↗

NASA NTRS1988

Pressure induced ageing of polymers

The nonlinearly viscoelastic response of an amorphous homopolymer is considered under aspects of time dependent free volume behavior. In contrast to linearly viscoelastic solids, this model couples shear and volume deformation through a shift function which influences the rate of molecular relaxation or creep. Sample computations produce all those qualitative features one observes normally in uniaxial tension including the rate dependent formation of a yield point as a consequence of the history of an imposed pressure.

Emri, I.↗

DOE OSTI2024

A Spectacular Viscoelastic Model Calibration for 828/D230/Alox Generated from Legacy Sandia Data

The nonlinear viscoelastic Spectacular model is calibrated to the thermo-mechanical behavior of 828/D230/Alox with an alox volume fraction of 20 %. Legacy experimental data from Sandia’s polymer properties database (PPD) is used to calibrate the model. Based on known densities of the epoxy 828/D230 and the alox filler, the alox volume fractions listed on the PPD were likely reported incorrectly. The alox volume fractions are recalculated here. Using the recalculated alox volume fractions, the PPD contains experimental data for 828/D230/Alox with alox volume fractions of 16 %, 24 %, and 33 %, so the thermo-mechanical behavior at 20 % alox volume fraction is estimated by interpolating between the bounding cases of of 16 % and 24 %. Because the Spectacularmodel can be fairly challenging to calibrate, the calibration procedure is described in detail. Several of the calibration steps involve inverse parameter identification, where an experiment is simulated and parameters are iteratively updated until the model response matches the experimental data. As the PPD does not fully describe all experimental procedures, the experimental simulations use assumed thermal and mechanical loading rates that are typical for the viscoelastic characterization of epoxies. Spectacular uses four independent relaxation functions related to volumetric (ƒ 1 ), shear (ƒ 2 ), thermal strain (ƒ 3 ), and thermal relaxations (ƒ 4 ). The previous SPEC model form, also known as the universal_polymer model, uses two independent relaxation functions related to volumetric and thermal relaxation (ƒ ν = ƒ 1 = ƒ 3 = ƒ 4 ) and shear relaxation (ƒ s = ƒ 2 ). The two constitutive choices are briefly evaluated here, where it is found that the four relaxation function approach of Spectacular was better suited for fitting the coefficient of thermal expansion during both heating and cooling.

36 MATERIALS SCIENCE↗

DOE OSTI2026

Characterization of ceramic fuel powder packing fractions to support INFLUX

Triply periodic minimal surface (TPMS)-based structures show marked potential in novel nuclear reactor fuel designs, as their high surface area-to-volume ratio increases the efficiency of heat transfer out of the fuel, enabling safer, more innovative reactor designs. This milestone report addresses the role of dUO 2 powder processing route on the fill behavior of TPMS-based cladding shells to understand and advance the feasibility of manufacturing TPMS-based nuclear fuel forms. dUO 2 powder was processed through either a dry granulation route, varying consolidation pressure, or through milling, varying milling time, milling method and milled size distribution. The lowest tapped bulk densities (TBD), but best powder flowabilities, were obtained when testing unprocessed dUO 2 powder which was prone to self-agglomeration and formed low-density spheroids. The highest TBD and lowest flowabilities were obtained when using powder produced by hammer-milling dUO 2 powder to pass through a 200-mesh sieve, which led to particles with angular morphologies. Powder produced by dry granulation exhibited TBD that varied according to the consolidation pressure used to form the initial pellets and exhibited improved flowabilities when compared to hammer-milled material. Because of the large span of granule sizes formed as well as the irregular shape associated with the granules, a packing fraction of 0.69 was achieved, exceeding the analytical solution for random close packing of mono-sized spheres. TPMS polymer shells were loaded with unprocessed, granulated, and hammer-milled dUO 2 powders, and their qualitative packing behaviors were analyzed using x-ray computed tomography (xCT). TBDs calculated after loading TPMS polymer shells were 10-20% lower when compared to tapped bulk density measurements taken in a glass graduated cylinder, indicating a non-trivial impact on the tapped bulk density of either the TPMS channel size, TPMS channel surface material, powder cohesiveness, or a combination of the two parameters. A metallic zircaloy-4 TPMS shell will be loaded with hammer-milled dUO 2 powder upon receipt of the shell from Oak Ridge National Laboratory (ORNL) and shipped to Idaho National Labs (INL) for subsequent hot isostatic pressing (HIP) densification experiments.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2022

Variable-Temperature Scattering and Spectroscopy Characterizations for Temperature-Dependent Solution Assembly of PffBT4T-Based Conjugated Polymers

The solution structure of conjugated polymers (CPs) from which the films are cast is critical for tailoring the thin-film morphology thus device performance. Here, we used multimodal variable-temperature scattering and spectroscopy tools to fully quantify the solution assembly of poly[(5,6-difluoro-2,1,3-benzothiadiazol-4,7-diyl)-alt-(3,3'''-dialkyl-2,2';5',2'';5'',2'''-quaterthiophen-5,5'''-diyl)] (PffBT4T) polymers with varying side-chain lengths at different assembly temperatures. The conformational and aggregation behaviors for PffBT4T-based CPs were found to be very sensitive to both temperature and side chain length using ultraviolet–visible (UV–vis) spectroscopy, nuclear magnetic resonance (NMR) spectroscopy, dynamic light scattering (DLS), and small-angle neutron scattering (SANS). We found that with slightly increasing side chain length from 2-octyldodecyl (C8C12) to 2-nonyltridecyl (C9C13), PffBT4T-based CPs show a significant decrease in aggregation-to-dissolved chain transition temperature (10 °C), degree of aggregation, enthalpy change of aggregation, and size of the aggregates in solution. At room temperature, PffBT4T polymer strongly aggregated to form fabric structure with the film thickness of a few nanometers in thickness and hundreds of nanometers in length, as probed by atomic force microscopy (AFM), transmission electronic microscopy (TEM), and dynamic light scattering (DLS). At the elevated temperature above the aggregation-to-dissolved chain transition temperature, PffBT4T is fully dissolved and adopts a semiflexible coil conformation with the persistence length of 3.1 nm for PffBT4T-C8C12 and a slightly increased persistence length of 3.4 nm for PffBT4T-C9C13, according to temperature-dependent SANS measurements. Longer side chains of PffBT4T-C9C13 also lead to less aggregation enthalpy gain compared with PffBT4T-C8C12. This work provides a solution structure manipulating strategy of CPs and thus will inspire the molecular design and processing protocols of CPs toward higher performance electronic devices.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Symmetry-Breaking and Self-Sorting in Block Copolymer-Based Multicomponent Nanocomposites

Co-assembly of inorganic nanoparticles (NPs) and nanostructured polymer matrix represents an intricate interplay of enthalpic or entropic forces. Particle size largely affects the phase behavior of the nanocomposite. Theoretical studies indicate that new morphologies would emerge when the particles become comparable to the soft matrix's size, but this has rarely been supported experimentally. By designing a multicomponent blend composed of NPs, block copolymer-based supramolecules, and small molecules, a 3-D ordered lattice beyond the native BCP's morphology was recently reported when the particle is larger than the microdomain of BCP. The blend can accommodate various formulation variables. In this work, when the particle size equals the microdomain size, a symmetry-broken phase appears in a narrow range of particle sizes and compositions, which we named the "train track" structure. In this phase, the NPs aligned into a 3-D hexagonal lattice and packed asymmetrically along the c axis, making the projection of the ac and the bc plane resemble train tracks. Computational studies show that the broken symmetry reduces the polymer chain deformation and stabilizes the metastable hexagonally perforated lamellar morphology. Given the mobility of the multicomponent blend, the system shows a self-sorting behavior: segregating into two macroscopic phases with different nanostructures based on only a few nanometers NP size differences. Smaller NPs form "train track" morphology, while larger NPs form a "simple hexagon" structure, where the NPs take a symmetric hexagonal arrangement. Detailed structural evolution and simulation studies confirm the systematic-wide cooperativity across different components, indicating the strong self-regulation of the multicomponent system.

"train track" morphology↗

DOE OSTI2026

Tuning the Mechanical Properties of Crosslinked Copolymers via Sequence and Solvent‐Selective Swelling for Vat Photopolymerization

Block copolymers (BCPs) offer distinct advantages for vat photopolymerization by enabling mechanically programmable network structures through microphase-separated morphologies that can be kinetically trapped during curing, yielding properties unattainable in homogeneous resins. However, the respective roles of repeat-unit sequence and solvent environment, together with their interplay in directing network formation and mechanical performance, remain unclear. Here, we synthesize a series of CO 2 -based polycarbonate copolymers comprising a crosslinkable glassy poly(vinyl cyclohexene carbonate) (PVCHC, A block) and a non-crosslinkable soft poly(propylene carbonate) (PPC, B block). The polymer sequence is systematically varied (ABA, BAB, and statistical), and solvent choice controls block-selective swelling to jointly control gelation behavior, microphase morphology, and mechanical response through changes in the accessibility and local environment of photocrosslinkable vinyl groups during network formation, as revealed by photorheology and small angle x-ray scattering. By tuning polymer sequence and curing solvent, we transform nominally identical formulations from brittle to highly ductile materials, achieving a three-orders-of-magnitude range in toughness (0.003 to 9.1 MJ m −3 ). These results establish clear structure–processing–property relationships and identify polymer sequence and selective solvation as powerful strategies for programming both printability and performance of block copolymer resins for additive manufacturing.

additive manufacturing↗