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All sourcesNASA NTRSDOE OSTI
NASA NTRS2005

NASA Tech Briefs, September 2005

Topivs include: Diamond-Coated Carbon Nanotubes for Efficient Field Emission; Improved Anode Coatings for Direct Methanol Fuel Cells; Advanced Ablative Insulators and Methods of Making Them; PETIs as High-Temperature Resin-Transfer-Molding Materials; Stable Polyimides for Terrestrial and Space Uses; Low-Density, Aerogel-Filled Thermal-Insulation Tiles; High-Performance Polymers Having Low Melt Viscosities; Nonflammable, Hydrophobic Aerogel Composites for Insulation; Front-Side Microstrip Line Feeding a Raised Antenna Patch; Medium-Frequency Pseudonoise Georadar; Facilitating Navigation Through Large Archives; Program for Weibull Analysis of Fatigue Data; Comprehensive Micromechanics-Analysis Code - Version 4.0; Component-Based Visualization System; Software for Engineering Simulations of a Spacecraft; LabVIEW Interface for PCI-SpaceWire Interface Card; Path Following with Slip Compensation for a Mars Rover; International Space Station Electric Power System Performance Code-SPACE; Software for Automation of Real-Time Agents, Version 2; Software for Optimizing Plans Involving Interdependent Goals; Computing Gravitational Fields of Finite-Sized Bodies; Custom Sky-Image Mosaics from NASA's Information Power Grid; ANTLR Tree Grammar Generator and Extensions; Generic Kalman Filter Software; Alignment Stage for a Cryogenic Dilatometer; Rugged Iris Mechanism; Treatments To Produce Stabilized Aluminum Mirrors for Cryogenic Uses; Making AlNx Tunnel Barriers Using a Low-Energy Nitrogen-Ion Beam; Making Wide-IF SIS Mixers with Suspended Metal-Beam Leads; Sol-Gel Glass Holographic Light-Shaping Diffusers; Automated Counting of Particles To Quantify Cleanliness; Phase Correction for GPS Antenna with Nonunique Phase Center; Compact Infrasonic Windscreen; Broadband External-Cavity Diode Laser; High-Efficiency Solar Cells Using Photonic-Bandgap Materials; Generating Solid Models from Topographical Data; Computationally Lightweight Air-Traffic-Control Simulation; Spool Valve for Switching Air Flows Between Two Beds; Partial Model of Insulator/ Insulator Contact Charging; Asymmetric Electrostatic Radiation Shielding for Spacecraft; and Reusable Hybrid Propellant Modules for Outer-Space Transport.

Source record↗
NASA NTRS2009

Recent Advances in Thermoplastic Puncture-Healing Polymers

Self-healing materials provide a route for enhanced damage tolerance in materials for aerospace applications. In particular, puncture-healing upon impact has the potential to mitigate significant damage caused by high velocity micrometeoroid impacts. This type of material also has the potential to improve damage tolerance in load bearing structures to enhance vehicle health and aircraft durability. The materials being studied are those capable of instantaneous puncture healing, providing a mechanism for mechanical property retention in lightweight structures. These systems have demonstrated healing capability following penetration of fast moving projectiles -- velocities that range from 9 mm bullets shot from a gun (approx.330 m/sec) to close to micrometeoroid debris velocities of 4800 m/sec. In this presentation, we report on a suite of polymeric materials possessing this characteristic. Figure 1 illustrates the puncture healing concept. Puncture healing in these materials is dependent upon how the combination of a polymer's viscoelastic properties responds to the energy input resulting from the puncture event. Projectile penetration increases the temperature in the vicinity of the impact. Self-healing behavior occurs following puncture, whereby energy must be transferred to the material during impact both elastically and inelastically, thus establishing two requirements for puncture healing to occur: a.) The need for the puncture event to produce a local melt state in the polymer material and b.) The molten material has to have sufficient melt elasticity to snap back and close the hole. 1,2 Previous ballistic testing studies revealed that Surlyn materials warmed up to a temperature approx.98 C during projectile puncture (3 C higher than it s melting temperature). 1,2 The temperature increase produces a localized flow state and the melt elasticity to snap back thus sealing the hole. Table 1 lists the commercially polymers studied here, together with their physical properties. The polymers were selected based on chemical structure, tensile strengths, tensile moduli, glass transition temperature, melting temperatures, and impact strength. The thermal properties of the polymers were characterized by Differential Scanning Calorimetry (DSC) and Dynamic Mechanical Analysis (DMA). Mechanical properties were assessed by a Sintech 2W instron according to ASTM D1708 or D638 at crosshead speeds of 5.08 cm/min. 7.6 cm x 7.6 cm panels of the different materials were prepared and ballistic testing was performed at various temperatures. The panels were shot with a .223 caliber semiautomatic rifle from a distance of 23 meters at various temperatures. Chronographs were used to measure initial and final bullet velocity. Temperatures at the site of impact were measured using a FLIR ThermaCAM S60 thermal camera. A Vision Research model Phantom 9 high speed video camera was used to capture high speed video footage of ballistics testing.

Gordon, K. L.↗
DOE OSTI2021

Joining Light Metals with Polymer Composites Through Metal Overcasting

This work investigates a unique technique to join aluminum (Al) and magnesium (Mg) alloys to carbon fiber reinforced polymer (CFRP) composites without the use of adhesives or mechanical fasteners. The joints were made using an overcasting technique where the molten alloys were cast around the polymer composites using high pressure die casting method. Rapid cooling during casting allowed the composite to be embedded inside the cast metal without causing any gross damage to the former even though the molten metal temperature exceeded the melting point of the composite matrix by several 100’s of deg. C. The metal/composite interface was examined using optical microscopy and x-ray imaging and the joint strength was examined through tensile testing. Although evidence of polymer melting was evident in the x-ray images, the embedded section of the composite coupons retained their overall shape and integrity. Preliminary tension tests on Al/CFRP composites showed strength degradation of the CFRP and it failed near the metal/CFRP interface (outside the joint). Strength degradation in the CFRP suggests that the overcasting process needs further optimization to minimize thermal excursion in the CFRP. Nevertheless, the overcasting process shows great promise as a unique joining technique with application in fabricating light-weight structures for automotive and transportation industries.

overcasting, Casting, Mg Castings, Al Casting, Joi↗
NASA NTRS2004

Characterization of Composite Fan Case Resins

The majority of commercial turbine engines that power today s aircraft use a large fan driven by the engine core to generate thrust which dramatically increases the engine s efficiency. However, if one of these fan blades fails during flight, it becomes high energy shrapnel, potentially impacting the engine or puncturing the aircraft itself and thus risking the lives of passengers. To solve this problem, the fan case must be capable of containing a fan blade should it break off during flight. Currently, all commercial fan cases are made of either just a thick metal barrier or a thinner metal wall surrounded by Kevlar-an ultra strong fiber that elastically catches the blade. My summer 2004 project was to characterize the resins for a composite fan case that will be lighter and more efficient than the current metal. The composite fan case is created by braiding carbon fibers and injecting a polymer resin into the braid. The resin holds the fibers together, so at first using the strongest polymer appears to logically lead to the strongest fan case. Unfortunately, the stronger polymers are too viscous when melted. This makes the manufacturing process more difficult because the polymer does not flow as freely through the braid, and the final product is less dense. With all of this in mind, it is important to remember that the strength of the polymer is still imperative; the case must still contain blades with high impact energy. The research identified which polymer had the right balance of properties, including ease of fabrication, toughness, and ability to transfer the load to the carbon fibers. Resin deformation was studied to better understand the composite response during high speed impact. My role in this research was the testing of polymers using dynamic mechanical analysis and tensile, compression, and torsion testing. Dynamic mechanical analysis examines the response of materials under cyclic loading. Two techniques were used for dynamic mechanical analysis. The ARES Instrument analyzed the material through torsion. The second machine, TA Instruments apparatus, applied a bending force to the specimen. These experiments were used to explore the effects of temperature and strain rate on the stiffness and strength of the resins. The two different types of loading allowed us to verify our results. An axial-torsional load frame, manufactured by MTS Systems, Inc., was used to conduct the tensile, compression, and torsional testing. These tests were used to determine the stress-strain curves for the resins. The elastic and plastic deformation data was provided to another team member for characterization of high fidelity material property predictions. This information was useful in having a better understanding of the polymers so that the fan cases could be as sturdy as possible. Deformation studies are the foundation for the computational modeling that provides the structural design of a composite engine case as well as detailed analysis of the blade impact event.

Dvoracek, Charlene M.↗
DOE OSTI2024

Chain dynamics of alternating polymers P(C n EG 4 )

Alternating or sequence defined polymers attract the attention of an increasing number of researchers recently. Due to their different blocks, they are very customizable and material properties can be tuned. In this publication, we present dynamical studies with focus on polymer dynamics, investigated by rheology and fast field cycling (FFC) NMR. The molecular weight dependencies of the relaxation time and zero-shear viscosity could hint to entanglement effects; however, the spectral shape of the viscoelastic data resembles the polymer dynamics of unentangled melts. Furthermore, taking both techniques into account, i.e. rheology and FFC NMR leads to the conclusion that the relaxation spectra of the alternating polymer are similar to those of linear polymers.

36 MATERIALS SCIENCE↗
NASA NTRS2013

Applications for Gradient Metal Alloys Fabricated Using Additive Manufacturing

Recently, additive manufacturing (AM) techniques have been developed that may shift the paradigm of traditional metal production by allowing complex net-shaped hardware to be built up layer-by-layer, rather than being machined from a billet. The AM process is ubiquitous with polymers due to their low melting temperatures, fast curing, and controllable viscosity, and 3D printers are widely available as commercial or consumer products. 3D printing with metals is inherently more complicated than with polymers due to their higher melting temperatures and reactivity with air, particularly when heated or molten. The process generally requires a high-power laser or other focused heat source, like an electron beam, for precise melting and deposition. Several promising metal AM techniques have been developed, including laser deposition (also called laser engineered net shaping or LENS® and laser deposition technology (LDT)), direct metal laser sintering (DMLS), and electron beam free-form (EBF). These machines typically use powders or wire feedstock that are melted and deposited using a laser or electron beam. Complex net-shape parts have been widely demonstrated using these (and other) AM techniques and the process appears to be a promising alternative to machining in some cases. Rather than simply competing with traditional machining for cost and time savings, the true advantage of AM involves the fabrication of hardware that cannot be produced using other techniques. This could include parts with "blind" features (like foams or trusses), parts that are difficult to machine conventionally, or parts made from materials that do not exist in bulk forms. In this work, the inventors identify that several AM techniques can be used to develop metal parts that change composition from one location in the part to another, allowing for complete control over the mechanical or physical properties. This changes the paradigm for conventional metal fabrication, which relies on an assortment of "post-processing" methods to locally alter properties (such as coating, heat treating, work hardening, shot peening, etching, anodizing, among others). Building the final part in an additive process allows for the development of an entirely new class of metals, so-called "functionally graded metals" or "gradient alloys." By carefully blending feedstock materials with different properties in an AM process, hardware can be developed with properties that cannot be obtained using other techniques but with the added benefit of the net-shaped fabrication that AM allows.

Hofmann, Douglas C.↗
DOE OSTI2024

Evaluating Iodine Immobilization Technologies: Cermets, Polycermets, and Polyhalmets

The work in this report documents the efforts conducted to assess the feasibility of some of the ideas documented in Pacific Northwest National Laboratory invention disclosure reports (IDRs) including: 1) Iodine capture in polyacrylonitrile (PAN)-containing composite sorbents (32451-E). In this work, the composites evaluated included Ag0, Bi0, Cu0, Bi2S3, and Cu2S embedded in PAN. 2) Metal iodide removal from these sorbents through dissolution in dimethyl sulfoxide (DMSO) (32729-E). In this work, PAN dissolution was evaluated for multiple types of sorbents including Ag-Pan, Bi-PAN, Cu-PAN, Bi2S3-PAN, and Cu2S-PAN. 3) Using metal-sulfide sorbents for iodine capture (32647-E). In this work, the composites evaluated under this IDR included Ag2S, Bi2S3, and Cu2S embedded in PAN. 4) Using low-melting metals to immobilize (encapsulate) iodine-loaded and polymer-containing sorbents into polymer-ceramic-metal (called polycermet) or polymer-halide-metal (called polyhalmet) composite waste forms (32625-E). In this work, the iodine-loaded PAN composites included AgI-PAN, BiI-PAN, and CuI-PAN. 5) Ceramic-metal composite waste form synthesis of polymer-containing materials using low-melting metals like bismuth, tin, or bismuth-tin alloys (32537-E). In this work, the metals evaluated included Bi, 58Bi-42Sn eutectic. 6) Cermets for immobilizing commercial sorbents loaded with radioiodine (32806-E). In this work, AgIX (iodine-loaded silver faujasite zeolite) was evaluated in cermet form.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗
DOE OSTI2024

The effect of stretching on polyamide – 6: assessment of crystallinity, mechanical properties, and surface roughness

Polyamide-6 (PA6), or nylon-6, is a widely used low-cost polymer material for various applications. Manufacturing PA6 into fibers involves a spinning process such as melt extrusion, which orients the polymer chains into a semicrystalline structure. When stretching the produced fibers to high strains, the PA6 fibers transition the metastable gamma phase back into the stable gamma phase. The effects of these large stretches on mechanical properties have not been explored after the stretch has been released. In this study, the effects on mechanical properties were studied by stretching the PA6 fibers from 10% to 50% tensile strain and subsequently releasing the fibers. The stretched fibers were characterized by X-ray diffraction and atomic force microscopy to determine the changes to the crystal structure and surface roughness. The stretched fibers were then tensile tested to failure and the tensile properties were examined. The stress-strain curves on the post-stretched PA6 fibers showed clear softening in the fibers with lower initial moduli after 30% stretching. Furthermore, these results may hold a clue to softening of fibers in applications with repeated loading and have implications for mechanical stability and fatigue of this polymeric material.

36 MATERIALS SCIENCE↗
NASA NTRS1988

The development of two new KC-135 furnaces for studies on microgravity materials processing

Wyle Laboratories is currently designing and fabricating two KC-135 materials processing furnaces for Marshall Space Flight Center. The first of these, called the Rapid Melt/Rapid Quench (RM/RQ) Furnace, will be used to melt and resolidify Cu-, Al-, and Ni-based alloys and composites, all during the 20 to 30 seconds of low gravity (0.1 to 0.001 g) available in a single parabola of the KC-135. In addition, it will be capable of directional solidification of these alloys. The furnace can be configured for either liquid or gas quenching of the samples. The second furnace, called the Polymer Solidification Transparent (PST) Furnace, will use a wide range of sample translation rates to directionally solidify polymers and low-melting-point metals as the KC-135 flies a series of parabolic maneuvers. The use of transparent crucibles and an optics system between the hot and cold zones of the furnace will allow for high-resolution video monitoring of the solid-liquid interface during processing. It is hoped that the development of these two furnaces will lead to significant increases in understanding of interface kinetics, fluid flow, and heat transfer in materials during solidification in a low-gravity environment.

Fiske, Michael↗
DOE OSTI2026

Closed‐Loop Recycling of Poly(pentylene Adipate‐ co ‐Terephthalate) via Amine‐Catalyzed Methanolysis

Advancing circularity through effective chemical recycling strategies is essential for enabling the sustainable use of emerging biodegradable polyesters in film applications. In this context, poly(pentylene adipate-co-terephthalate) with a 40/60 adipate-to-terephthalate ratio (PPeAT60), a significantly stiffer and partially biobased copolyester recently reported by our team, offers improved mechanical performance and processability compared to commercial poly(butylene adipate-co-terephthalate), while providing a platform to evaluate advanced recycling approaches for film applications. Here, this study describes depolymerization of PPeAT60 through amine-catalyzed methanolysis, followed by the repolymerization of the recovered monomers. The resulting repolymerized material exhibited a molar mass distribution, chemical structure, and thermal stability comparable to the virgin polymer, confirming the technical feasibility of the methanolysis-based recycling route. Both polymers displayed nearly identical melting, glass transition, and decomposition temperatures, crystallinity, and modulus, demonstrating full structural and mechanical reproducibility after recycling. Variations in crystallization kinetics, elongation at break, and barrier properties likely arise from trace impurities (<1%) introduced during processing acting as nucleating and stress-inducing agents. Overall, these results demonstrate that PPeAT60 retains its key properties after chemical recycling, establishing methanolysis as a promising platform for recycling of this partially biobased polymer that may be able to replace both conventional polyolefins and PBAT in flexible packaging applications.

09 BIOMASS FUELS↗
DOE OSTI2021

Morphology and Dynamics of Bottlebrush Polymers

This thesis makes significant advances to the understanding of bottlebrush polymers. While bottlebrushes have received much attention due to the recent discovery of their unprecedented properties, including supersoftness, ultra-low viscosity, and hyperelasticity, this thesis is the first fundamental investigation at the molecular level that comprises structure and dynamics. Neutron scattering experiments, detailed within, reveal spherical or cylindrical shapes, instead of a random coil conformation. Another highlight is the analysis of the fast dynamics at the sub nm-length scale. The combination of three neutron spectrometers and the development of a new analysis technique enabled the calculation of the mean-square displacement over seven orders of magnitude in time scale. This unprecedented result can be applied to a broad class of samples, including polymers and other materials. The thesis is accessible to scientists from other fields, provides the reader with easily understandable guidelines for applying this analysis to other materials, and has the potential to make a significant impact on the analysis of neutron scattering data.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Dynamics of poly[n]catenane melts

Inspired by advances in the chemical synthesis of interlocking polymer architectures, extensive molecular dynamics simulations have been conducted to study the dynamical properties of poly[n]catenanes-polymers composed entirely of interlocking rings-in the melt state. Both the degree of polymerization (number of links) and the number of beads per ring are systematically varied, and the results are compared to linear and ring polymers. Herein, a simple Rouse-like model is presented, and its analytical solution suggests a decomposition of the dynamics into "ring-like" and "linear-like" regimes at short and long times, respectively. In agreement with this picture, multiple sub-diffusive regimes are observed in the monomer mean-squared-displacements even though interchain entanglement is not prevalent in the system. However, the Rouse-type model does not account for the topological effects of the mechanical bonds, which significantly alter the dynamics at intermediate length scales both within the rings and at the chain segment scales. The stress relaxation in the system is extremely rapid and may be conveniently separated into ring-like and linear-like contributions, again in agreement with the Rouse picture. However, the viscosity has a non-monotonic dependence on the ring size for long chains, which disagrees strongly with theoretical predictions. This unexpected observation cannot be explained in terms of chain disentanglement and is inconsistent with other measures of polymer relaxation. Possible mechanisms for this behavior are proposed and implications for materials design are discussed.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
NASA NTRS2011

Fire-Retardant Polymeric Additives

Polyhydroxyamide (PHA) and polymethoxyamide (PMeOA) are fire-retardant (FR) thermoplastic polymers and have been found to be useful as an additive for imparting fire retardant properties to other compatible, thermoplastic polymers (including some elastomers). Examples of compatible flammable polymers include nylons, polyesters, and acrylics. Unlike most prior additives, PHA and PMeOA do not appreciably degrade the mechanical properties of the matrix polymer; indeed, in some cases, mechanical properties are enhanced. Also, unlike some prior additives, PHA and PMeOA do not decompose into large amounts of corrosive or toxic compounds during combustion and can be processed at elevated temperatures. PMeOA derivative formulations were synthesized and used as an FR additive in the fabrication of polyamide (PA) and polystyrene (PS) composites with notable reduction (>30 percent for PS) in peak heat release rates compared to the neat polymer as measured by a Cone Calorimeter (ASTM E1354). Synergistic effects were noted with nanosilica composites. These nanosilica composites had more than 50-percent reduction in peak heat release rates. In a typical application, a flammable thermoplastic, thermoplastic blend, or elastomer that one seeks to render flame-retardant is first dry-mixed with PHA or PMeOA or derivative thereof. The proportion of PHA or PMeOA or derivative in the mixture is typically chosen to lie between 1 and 20 weight percent. The dry blend can then be melt-extruded. The extruded polymer blend can further be extruded and/or molded into fibers, pipes, or any other of a variety of objects that may be required to be fire-retardant. The physical and chemical mechanisms which impart flame retardancy of the additive include inhibiting free-radical oxidation in the vapor phase, preventing vaporization of fuel (the polymer), and cooling through the formation of chemical bonds in either the vapor or the condensed phase. Under thermal stress, the cyclic hydroxyl/ methoxy component forms polybenzoxazole (PBO) in a reaction that absorbs heat from its surroundings. PBO under thermal stress cross-links, forming a protective char layer, which thermally insulates the polymer. Thus, the formation of the char layer further assists to extinguish the fire by preventing vaporization of the polymeric fuel.

Williams, Martha K.↗
DOE OSTI2025

Material Extrusion Printing of Poly(Acrylonitrile‐Styrene‐Acrylate) and Poly(Acrylonitrile‐Butadiene‐Styrene) Structures Reinforced with Poly(Phenylene Oxide) Additives for Improved Thermomechanical Properties and their Surface Analysis by Time‐of‐Flight Secondary Ion Mass Spectrometry

Fused filament fabrication offers the ability to 3D print complex geometries made from plastic filament materials; however, these parts are mechanically outperformed by parts created by traditional fabrication methods. To overcome this challenge, a high-performance polymer poly(2,6-dimethyl-1,4-phenylene oxide) (PPO) is incorporated as an additive into two common engineering thermoplastics, poly(acrylonitrile-styrene-acrylate) (ASA) and poly(acrylonitrile-butadiene-styrene) (ABS). Structures printed from these polymer blends are more mechanically robust compared to those prepared from the parent polymers, with low loading levels (1–5 wt%) of PPO improving the elastic strength by up to ≈30% relative to the parent terpolymers. Even at higher loading levels (10 and 20 wt% PPO), there is no evidence of additive aggregation in the model thin films, which is supported by compositional analysis of the copolymers and chemical analysis via time-of-flight secondary ion mass spectrometry. The enhancements in mechanical properties of ASA and ABS blends appear to be a consequence of homogeneous incorporation of the PPO additive. In conclusion, this work explores expanding materials-property space using miscible blends of engineering thermoplastics to improve mechanical performance as a general approach to overcoming challenges with parts created by melt-based material extrusion printing.

additive manufacturing↗
DOE OSTI2025

Confocal Raman Microscopy for Measuring In Situ Temperature-Dependent Structural Changes in Poly(Ethylene Oxide) Thin Films

Crystallization from the melt is a critical process governing the properties of semi-crystalline polymeric materials. While structural analyses of melting and crystallization transitions in bulk polymers have been widely reported, in contrast, those in thin polymer films on solid supports have been underexplored. Herein, in situ Raman microscopy and self-modeling curve resolution (SMCR) analysis are applied to investigate the temperature-dependent structural changes in poly(ethylene oxide) (PEO) films during melting and crystallization phase transitions. By resolving complex overlapping sets of spectra, SMCR analysis reveals that the thermal transitions of 50 µm thick PEO films comprise two structural phases: an ordered crystalline phase and a disordered amorphous phase. The ordered structure of the crystalline PEO film entirely disappears as the polymer is heated; conversely, the disordered structure of the amorphous PEO film reverts to the ordered structure as the polymer is cooled. Broadening of the Raman bands was observed in PEO films above the melting temperature (67 °C), while sharpening of bands was observed below the crystallization temperature (45 °C). The temperatures at which these spectral changes occurred were in good agreement with differential scanning calorimetry (DSC) measurements, especially during the melting transition. The results illustrate that in situ Raman microscopy coupled with SMCR analysis is a powerful approach for unraveling complex structural changes in thin polymer films during melting and crystallization processes. Furthermore, we show that confocal Raman microscopy opens opportunities to apply the methodology to interrogate the structural features of PEO or other surface-supported polymer films as thin as 2 µm, a thickness regime beyond the reach of conventional thermal analysis techniques.

Koh, Miharu [Department of Chemistry, University o↗
DOE OSTI2022

A case study of high-temperature polyetherimide film capacitor fabrication

Capacitors, as the basic building block of power electronics and electrical systems, are the major constraint of the increasingly integrated power systems that require new capable polymer dielectric films operating at higher temperatures >125 °C. Despite tremendous research efforts on the lab scale, there remains a considerable barrier and knowledge basis for converting polymeric films to functioning capacitors desired in actual applications. Here, the authors tackled the polyetherimide (PEI) film scale up issues and developed various engineering processes for film de-wrinkling, optimal metallization, static elimination, and capacitor fabrication improvement. The authors discovered various fabrication challenges such as the electrostatic charge, metallization scheme, winding tension, and end electrode disconnects. To fabricate a high yield of PEI capacitor bobbins, it is necessary to utilize static eliminators (radioactive ionizers), moderately thick aluminum metallization (15–30 Ω/sq), and winding tension (60–100 g). It is also effective to evaluate capacitance, dielectric loss, equivalent series resistance, and thermal cycling stability of capacitors. This work sheds some light on converting PEI films and other polymeric films to capacitors on a scale up fabrication effort. The practical learning from film handling to capacitor fabrication in this work provided the necessary knowledge for manufacturing high-temperature polar film capacitors.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Engineering lithium-ion battery cathodes for high-voltage applications using electromagnetic excitation

Microwave radiation (MWR), a type of electromagnetic excitation source, reduces the synthesis temperature and processing time for chemical reactions compared to traditional synthesis methods. Recently, we demonstrated that MWR can engineer ceramics with different crystal phases compared to traditional methods [ Journal of Materials Chemistry A 5 , 35 (2017)]. Here, we further apply the MWR-assisted technique to improve the electrochemical performance of LiCoO 2 cathodes by engineering TiO 2 and ZrO 2 ceramic coatings. Electrochemical tests suggest that the TiO 2 coating improves the rate capability of the LiCoO 2 electrode. Both TiO 2 and ZrO 2 coatings improve the high-voltage (4.5 V) cycling stability of LiCoO 2 . The capacity remaining is improved from 52.8 to 84.4% and 81.9% by the TiO 2 coating and the ZrO 2 coating, respectively, after 40 cycles. We compare these results with existing studies that apply traditional methods to engineer TiO 2 /ZrO 2 on LiCoO 2 , and find that the MWR-assisted method shows better performance improvement. X-ray photoelectron spectroscopy measurements suggest that the improved cycling stability arises from the formation of metal fluorides that protect the electrode from side reactions with electrolytes. This mechanism is further supported by the reduced Co dissolution from TiO 2 /ZrO 2 -coated LiCoO 2 electrode after cycling. This study provides a new toolbox facilitating the integration of many delicate, low melting point materials like polymers into battery electrodes.

25 ENERGY STORAGE↗
DOE OSTI2020

Cyclic Topology Enhancing Structural Ordering and Stability of Comb-Shaped Polypeptoid Thin Films against Melt-Induced Dewetting

We investigated the effect of cyclic chain topology on the molecular ordering and thermal stability of comb-shaped polypeptoid thin films on silicon (Si) substrates. Cyclic and linear poly(N-decylglycine) (PNDG) bearing long n-decyl side chains were synthesized by ring-opening polymerization of N-decylglycine-derived N-carboxyanhydrides. When the spin-coated thin films were subjected to thermal annealing at temperatures above the melting temperature (T > T m ), the cyclic PNDG films exhibited significantly enhanced stability against melt-induced dewetting than the linear counterparts (l-PNDG). When recrystallized at temperatures below the crystallization temperature (T < T c ), the homogeneous c-PNDG films exhibit enhanced crystalline ordering relative to the macroscopically dewetted l-PNDG films. Both cyclic and linear PNDG molecules adopt cis-amide conformations in the crystalline film, which transition into trans-amide conformations upon melting. A top-down solvent leaching treatment of both l/c-PNDG films revealed the formation of an irreversibly physisorbed monolayer with similar thickness (ca. 3 nm) on the Si substrate. The physisorbed monolayers are more disordered relative to the respective thicker crystalline films for both cyclic and linear PNDGs. Upon heating above T m , the adsorbed c-PNDG chains adopt trans-amide backbone conformation identical with the free c-PNDG molecules in the molten film. By contrast, the backbone conformations of l-PNDG chains in the adsorbed layers are notably different from those of the free chains in the molten film. We postulate that the conformational disparity between the chains in the physically adsorbed layers versus the free chains in the molten film is an important factor to account for the difference in the thermal stability of PNDG thin films. These findings highlight the use of cyclic chain topology to suppress the melt-induced dewetting in polymer thin films.

36 MATERIALS SCIENCE↗