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DOE OSTI2023

Understanding the Influence of Li 7 La 3 Zr 2 O 12 Nanofibers on Critical Current Density and Coulombic Efficiency in Composite Polymer Electrolytes

Composite polymer electrolytes (CPEs)are attractive materials for solid-state lithium metal batteries, owing to their high ionic conductivity from ceramic ionic conductors and flexibility from polymer components. As with all lithium metal batteries, however, CPEs face the challenge of dendrite formation and propagation. Not only does this lower the critical current density (CCD) before cell shorting, but the uncontrolled growth of lithium deposits may limit Coulombic efficiency (CE) by creating dead lithium. Here, we present a fundamental study on how the ceramic components of CPEs influence these characteristics. CPE membranes based on poly-(ethylene oxide) and lithium bis-(trifluoro methane sulfonyl)-imide(PEO-LiTFSI) with Li 7 La 3 Zr 2 O 12 (LLZO) nanofibers were fabricated with industrially relevant roll-to-roll manufacturing techniques. Galvanostatic cycling with lithium symmetric cells shows that the CCD can be tripled by including 50 wt % LLZO, but half-cell cycling reveals that this comes at the cost of CE. Varying the LLZO loading shows that even a small amount of LLZO drastically lowers the CE, from 88% at 0 wt % LLZO to 77% at just 2 wt % LLZO. Mesoscale modeling reveals that the increase in CCD cannot be explained by an increase in the macroscopic or microscopic stiffness of the electrolyte; only the microstructure of the LLZO nanofibers in the PEO-LiTFSI matrix slows dendrite growth by presenting physical barriers that the dendrites must push or grow around. This tortuous lithium growth mechanism around the LLZO is corroborated with mass spectrometry imaging. In conclusion, this work highlights important elements to consider in the design of CPEs for high-efficiency lithium metal batteries.

36 MATERIALS SCIENCE↗

NASA NTRS2014

2014 NEPP Tasks Update for Ceramic and Tantalum Capacitors

Presentation describes recent development in research on MnO2, wet, and polymer tantalum capacitors. Low-voltage failures in multilayer ceramic capacitors and techniques to reveal precious metal electrode (PME) and base metal electrode (BME) capacitors with cracks are discussed. A voltage breakdown technique is suggested to select high quality low-voltage BME ceramic capacitors.

ceramic capacitors↗

NASA NTRS2019

Materials and Processes for New Propulsion Systems with Reduced Environmental Impact

Aeronautics research at NASA Glenn Research Center includes development, characterization and modeling of high temperature, lightweight materials and fabrication processes for aircraft propulsion systems with increased efficiency and reduced emissions, fuel burn and noise. Current propulsion materials research includes Ceramic Matrix Composites and Environmental Barrier Coatings, Polymer Matrix Composites and Additive Manufacturing processes. This presentation will summarize recent progress and plans in these areas. Ceramic Matrix Composites for Turbine Components: As part of NASA's Aeronautics research, Glenn Research Center has developed Ceramic Matrix Composites for 2700 degrees Fahrenheit turbine engine applications in the next generation of ultra-efficient aircraft. In this presentation, the development of advanced fiber and matrix constituents that enabled this advancement will be reviewed, and characterization of the resulting improvements in mechanical properties and durability will be summarized. Progress toward the development and validation of models predicting the effects of the engine environment on durability of Ceramic Matrix Composites and Environmental Barrier Coatings will be summarized. Progress and plans for collaborative research with industry and other government agencies will be reviewed. Polymer Matrix Composites for Powertrain and Impact Protection: A lightweight, hybrid polymer matrix composite/steel gear concept for rotorcraft power transmission applications was evaluated at realistic speed, torque, and power conditions. Dynamic testing was performed at 5000 horsepower and 5400 revolutions per minute with no performance degradation. Test results demonstrated the potential of hybrid composite / metal gears to reduce gear weight by approximately 15 percent, enabling the implementation of multi-speed drive systems, which would otherwise have a weight penalty, for increased speed and efficiency. Results of post-test inspection and endurance tests will be presented. Separately, ballistic impact tests demonstrated improved damage tolerance in polymer matrix composites by incorporating lightweight, thermoplastic veil materials between selected composite plies during the composite fabrication process. Results of impact tests and post-test inspection will be presented. Additive Manufacturing for Electric Propulsion: Additive Manufacturing processes offer the potential to fabricate new, high power density electric motor designs with complex geometries, multi-material components and optimally designed components that would not be feasible with traditional manufacturing processes. High performance stator components using advanced 3-phase conductive coils were fabricated using direct printing with optimized silver pastes. Additional additive manufacturing methods are being used to fabricate rotors and motor housing components. Systems studies show that the higher performance and lower weight motors offer improved energy efficiency and reduced emissions. Improvements to motor performance resulting from optimized materials and component designs will be presented.

Additive Manufacturing↗

NASA NTRS1994

Controlled thermal expansion printed wiring boards based on liquid crystal polymer dielectrics

Dielectric materials based on innovative Liquid Crystal Polymers (LCP's) have been used to fabricate surface mount printed wiring boards (PWB's) with a coefficient of thermal expansion matched to leadless ceramic chip carriers. Proprietary and patented polymer processing technology has resulted in self reinforcing material with balanced in-plane mechanical properties. In addition, LCP's possess excellent electrical properties, including a low dielectric constant (less than 2.9) and very low moisture absorption (less than 0.02%). LCP-based multilayer boards processed with conventional drilling and plating processes show improved performance over other materials because they eliminate the surface flatness problems of glass or aramid reinforcements. Laser drilling of blind vias in the LCP dielectric provides a very high density for use in direct chip attach and area array packages. The material is ideally suited for MCM-L and PCMCIA applications fabricated with very thin dielectric layers of the liquid crystal polymer.

Knoll, Thomas E.↗

DOE OSTI2021

Powder diffraction

Powder diffraction is a non-destructive technique, which is experimentally simple in principle. Because the physics behind diffraction is well understood, an exceptionally large amount of information can be obtained from a single measurement. The positions and relative intensities of the peaks yield a fingerprint that can be used for qualitative phase analysis. Quantitative phase analysis can be obtained by detailed analysis of the intensities. Unit cells can be derived from the peak positions. Crystal structures can be solved using powder diffraction data and refined by the Rietveld method. The peak profiles contain information about crystallite size, strain and nanostructure. Non-idealities in the intensities give information on texture. Abandoning the crystallographic model provides information about local structure, by pair distribution function analysis. For powder diffraction, everything is a sample; the technique is commonly applied to characterize minerals, ceramics, metals and alloys, catalysts, polymers, pharmaceuticals, organic compounds, environmental and forensic samples, among others. The major features of contemporary laboratory powder diffractometers are described. Methods for obtaining suitable powder specimens are summarized. Major applications of qualitative and quantitative phase analysis, structure solution, size/strain/nanostructure analysis using peak profiles, texture analysis and pair distribution function analysis are introduced.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2020

Design of functional composite and all-inorganic nanostructured materials via infiltration of polymer templates with inorganic precursors

Robust and efficient approaches for the synthesis of materials with structure, porosity, and composition controlled at the nanoscale are highly important for a wide range of applications. Polymer templates are promising platforms to achieve such control. The self-assembly process of polymers provides access to diverse structures that can serve as templates for the deposition of inorganic materials. By infiltrating metal precursors from gas or liquid phases, using sequential infiltration synthesis (SIS) or swelling-based infiltration (SBI), respectively, into the polymer templates, one can create finely-tuned texturing of the surface films and bulk materials. In this review, we outline the specifics and dynamics of the polymer infiltration process and characterize the structure and properties of the synthesized materials. Finally, we highlight recent progress in implementing polymer infiltration-based nanoporous ceramics for many applications, including sensors, antireflective coatings, oil-absorbing foams, nanolithographic patterns, and catalytic materials.

Berman, Diana↗

NASA NTRS1999

Producing Fiber Reinforced Composites Having Dense Ceramic Matrices

A fiber preform is partially infiltrated with a ceramic material. A porous solid polymer is formed by reaction forming the infiltrated preform which is then pyrolized. Microporous carbon in the composite matrix is converted into silicon carbide.

Behrendt, Donald R.↗

NASA NTRS1998

Single-Transducer, Ultrasonic Imaging Method for High-Temperature Structural Materials Eliminates the Effect of Thickness Variation in the Image

NASA Lewis Research Center's Life Prediction Branch, in partnership with Sonix, Inc., and Cleveland State University, recently advanced the development of, refined, and commercialized an advanced nondestructive evaluation (NDE) inspection method entitled the Single Transducer Thickness-Independent Ultrasonic Imaging Method. Selected by R&D Magazine as one of the 100 most technologically significant new products of 1996, the method uses a single transducer to eliminate the superimposing effects of thickness variation in the ultrasonic images of materials. As a result, any variation seen in the image is due solely to microstructural variation. This nondestructive method precisely and accurately characterizes material gradients (pore fraction, density, or chemical) that affect the uniformity of a material's physical performance (mechanical, thermal, or electrical). Advantages of the method over conventional ultrasonic imaging include (1) elimination of machining costs (for precision thickness control) during the quality control stages of material processing and development and (2) elimination of labor costs and subjectivity involved in further image processing and image interpretation. At NASA Lewis, the method has been used primarily for accurate inspections of high temperature structural materials including monolithic ceramics, metal matrix composites, and polymer matrix composites. Data were published this year for platelike samples, and current research is focusing on applying the method to tubular components. The initial publicity regarding the development of the method generated 150 requests for further information from a wide variety of institutions and individuals including the Federal Bureau of Investigation (FBI), Lockheed Martin Corporation, Rockwell International, Hewlett Packard Company, and Procter & Gamble Company. In addition, NASA has been solicited by the 3M Company and Allison Abrasives to use this method to inspect composite materials that are manufactured by these companies.

Roth, Don J.↗

NASA NTRS2003

Characterization of a Ultra-high Temperature Ceramic Composite

Ultra-high temperature ceramics (UHTC) are of interest for hypersonic vehicle leading edge applications. Monolithic UHTCs are of concern because of their low fracture toughness and brittle behavior. UHTC composites (UHTCC) are being investigated as a possible approach to overcome these deficiencies. In this study a small sample of a UHTCC was evaluated by limited mechanical property tests, furnace oxidation exposures, and oxidation exposures in a flowing environment. The composite was prepared from a carbon fiber perform using ceramic particulates and a preceramic polymer. The as-received composite plate was non-uniform from front to back surface. Plate dimensions were 150 x 150 x 6 mm. The back surface had a fibrous, uniform appearance; XRD analysis revealed the presence of Sic and C. The front surface was smooth and non-uniform in appearance with evidence of a coarse grain structure produced by a liquid phase; XRD analysis revealed the presence of HfB2. Microcracks were present throughout the thickness as one might expect from a carbon fiber reinforced composite with attendant large thermal expansion mismatch between the matrix phases and the fibers. The HfB2 phase on the front surface was comparable in thickness to a fiber ply or about 0.6 mm, and surface microcracks were evident. Limited four point flexural tests were carried out at span to depth ratios of approximately 14 and 16 with markedly different results. Tests were run with the front or the back surface in tension. At the shorter span to depth failures occurred under a loading pin for both orientations. At a span to depth of 16 failures occurred in the center of the span with fracture clearly initiating from a tensile failure. Ultimate flexural strength, strain at ultimate stress, stress and strain at deviation from linear elastic behavior are reported. Strains at ultimate stress ranged from about 0.6 to 0.7 % for the back surface in tension, and 0.4 to 0.6 for the front surface in tension. At constant span to depth the strain at ultimate stress was about 0.2% greater for the back surface in tension and the ultimate strength was also higher. Strengths were in line with predictions from theory. Furnace oxidation studies were carried out at 1627 and 1927OC in a static furnace environment using ten minute cycles and one, five, and ten cycles. Limited oxidation studies were also carried out in a flowing oxyacetylene torch environment. Specimens were photographed, and weight and dimensional changes were determined. XRD and SEM characterizations were performed. Weight losses were attributed primarily to carbon fiber oxidation. The composite survived the torch test with little visible distress. Further details will be determined once metallographic studies are completed.

Levine, Stanley R.↗

NASA NTRS2020

Select Electronic Parts Operation at Extreme Low Temperature

The purpose of the study presented in this paper is to extend the test period of a selected set of electronics parts at cryogenic condition to dwell period of about 24 hours to demonstrate extreme cold operational capability of these components. The parts tested are tantalum polymer, BX and P90 type ceramic capacitors, thick film resistors, analog multiplexers, a digital inverter, and a D-flip-flop. These parts were tested to assist identifying candidate components that can be used for development of a cold capable telemetry board. There are several past investigations that have shown that COTS (commercial-off-the-shelf) capacitors and resistors tested at cryogenic temperatures and frequencies up to 10MHz did not exhibit significant changes in capacitance and resistance values. Also, there are several test results for active parts. These past tests collected measurements during a temperature sweep from room temperature down to cryogenic temperature with very short dwell time at cryogenic temperature, and back to room temperature. This study extends the operational dwell time to at least 24 hours and returning to room temperature operation without significant degradation in performance, thus, demonstrating the potential for longer dwell time in actual operation in these extreme cold temperatures and a method for identifying the cold operability.

Ashtijou, Mohammad↗

DOE OSTI2024

3D printing of ceramics: Advantages, challenges, applications, and perspectives

Abstract 3D printing (3DP) technologies have transformed the processing of advanced ceramics for small‐scale and custom designs during the past three decades. Simple and complex parts are designed and manufactured using 3DP technologies for structural, piezoelectric, and biomedical applications. Manufacturing simple or complex geometries or one‐of‐a‐kind components without part‐specific tooling saves significant time and creates new applications for advanced ceramic materials. Although development and innovations in 3DP of ceramics are far behind compared with metals or polymers, with the availability of different commercial machines in recent years for 3DP of ceramics, exponential growth is expected in this field in the coming decade. This article details various 3DP technologies for advanced ceramic materials, their advantages and challenges for manufacturing parts for various applications, and perspectives on future directions. We envision this work will be helpful to advanced ceramic researchers in industry and academia who are using different 3DP processes in the coming days.

36 MATERIALS SCIENCE↗

NASA NTRS1992

Approaches to polymer-derived CMC matrices

The use of polymeric precursors to ceramics permits the fabrication of large, complex-shaped ceramic matrix composites (CMC's) at temperatures which do not degrade the fiber. Processing equipment and techniques readily available in the resin matrix composite industry can be adapted for CMC fabrication using this approach. Criteria which influence the choice of candidate precursor polymers, the use of fillers, and the role of fiber architecture and ply layup are discussed. Three polymer systems, polycarbosilanes, polysilazanes, and polysilsesquioxanes, are compared as candidate ceramic matrix precursors.

Hurwitz, Frances I.↗

NASA NTRS1992

Approaches to polymer-derived CMC matrices

Hurwitz, Frances I.↗

NASA NTRS1996

Construction of a Piezoresistive Neural Sensor Array

The construction of a piezoresistive - piezoelectric sensor (or actuator) array is proposed using 'neural' connectivity for signal recognition and possible actuation functions. A closer integration of the sensor and decision functions is necessary in order to achieve intrinsic identification within the sensor. A neural sensor is the next logical step in development of truly 'intelligent' arrays. This proposal will integrate 1-3 polymer piezoresistors and MLC electroceramic devices for applications involving acoustic identification. The 'intelligent' piezoresistor -piezoelectric system incorporates printed resistors, composite resistors, and a feedback for the resetting of resistances. A model of a design is proposed in order to simulate electromechanical resistor interactions. The goal of optimizing a sensor geometry for improving device reliability, training, & signal identification capabilities is the goal of this work. At present, studies predict performance of a 'smart' device with a significant control of 'effective' compliance over a narrow pressure range due to a piezoresistor percolation threshold. An interesting possibility may be to use an array of control elements to shift the threshold function in order to change the level of resistance in a neural sensor array for identification, or, actuation applications. The proposed design employs elements of: (1) conductor loaded polymers for a 'fast' RC time constant response; and (2) multilayer ceramics for actuation or sensing and shifting of resistance in the polymer. Other material possibilities also exist using magnetoresistive layered systems for shifting the resistance. It is proposed to use a neural net configuration to test and to help study the possible changes required in the materials design of these devices. Numerical design models utilize electromechanical elements, in conjunction with structural elements in order to simulate piezoresistively controlled actuators and changes in resistance of sensors. The construction of these devices may show significant improvement in ability to interrogate signals and in the control of effective compliance. This work focuses on the development a variety of series/parallel interconnected piezoresistive control elements for the neural sensing function.

Carlson, W. B.↗

DOE OSTI2020

Enhanced Surface Interactions Enable Fast Li + Conduction in Oxide/Polymer Composite Electrolyte

Abstract Li + ‐conducting oxides are considered better ceramic fillers than Li + ‐insulating oxides for improving Li + conductivity in composite polymer electrolytes owing to their ability to conduct Li + through the ceramic oxide as well as across the oxide/polymer interface. Here we use two Li + ‐insulating oxides (fluorite Gd 0.1 Ce 0.9 O 1.95 and perovskite La 0.8 Sr 0.2 Ga 0.8 Mg 0.2 O 2.55 ) with a high concentration of oxygen vacancies to demonstrate two oxide/poly(ethylene oxide) (PEO)‐based polymer composite electrolytes, each with a Li + conductivity above 10 −4 S cm −1 at 30 °C. Li solid‐state NMR results show an increase in Li + ions (>10 %) occupying the more mobile A2 environment in the composite electrolytes. This increase in A2‐site occupancy originates from the strong interaction between the O 2− of Li‐salt anion and the surface oxygen vacancies of each oxide and contributes to the more facile Li + transport. All‐solid‐state Li‐metal cells with these composite electrolytes demonstrate a small interfacial resistance with good cycling performance at 35 °C.

Wu, Nan↗

NASA NTRS1989

Polymer derived Nicalon/Si-C-O composites - Processing and mechanical behavior

Ceramic matrix composites fabricated using Nicalon fiber and several polysilsesquioxane-derived Si-C-O matrices were characterized by optical and SEM and in four-point bending. In the matrix material linear shrinkages of up to 19 percent were observed for the vinylmethyl copolymer pyrolyzed to 1200 C, and up to 13 percent for the phenylmethyl material pyrolyzed to the same temperature, resulting in considerable matrix cracking. Under four-point loading, most composite samples fractured in a brittle manner as the result of strong fiber-matrix bonding. Flexural strengths, moduli, and ultimate strain varied with fiber sizing and processing parameters. Testing and analysis is being applied to promote more fibrous pullout during fracture.

Hurwitz, Frances I.↗

NASA NTRS2001

The Effect of Journal Roughness and Foil Coatings on the Performance of Heavily Loaded Foil Air Bearings

Foil air bearing load capacity tests were conducted to investigate if a solid lubricant coating applied to the surface of the bearing's top foil can function as a break-in coating. Two foil coating materials, a conventional soft polymer film (polyimide) and a hard ceramic (alumina), were independently evaluated against as-ground and worn (run-in) journals coated with NASA PS304, a high-temperature solid lubricant composite coating. The foil coatings were evaluated at journal rotational speeds of 30,000 rpm and at 25 C. Tests were also performed on a foil bearing with a bare (uncoated) nickel-based superalloy top foil to establish a baseline for comparison. The test results indicate that the presence of a top foil solid lubricant coating is effective at increasing the load capacity performance of the foil bearing. Compared to the uncoated baseline, the addition of the soft polymer coating on the top foil increased the bearing load coefficient by 120% when operating against an as-ground journal surface and 85 percent against a run-in journal surface. The alumina coating increased the load coefficient by 40% against the as-ground journal but did not have any affect when the bearing was operated with the run-in journal. The results suggest that the addition of solid lubricant films provide added lubrication when the air film is marginal indicating that as the load capacity is approached foil air bearings transition from hydrodynamic to mixed and boundary lubrication.

Radil, Kevin C.↗

NASA NTRS2011

Detection of Carbon Monoxide Using Polymer-Carbon Composite Films

A carbon monoxide (CO) sensor was developed that can be incorporated into an existing sensing array architecture. The CO sensor is a low-power chemiresistor that operates at room temperature, and the sensor fabrication techniques are compatible with ceramic substrates. Sensors made from four different polymers were tested: poly (4-vinylpryridine), ethylene-propylene-diene-terpolymer, polyepichlorohydrin, and polyethylene oxide (PEO). The carbon black used for the composite films was Black Pearls 2000, a furnace black made by the Cabot Corporation. Polymers and carbon black were used as received. In fact, only two of these sensors showed a good response to CO. The poly (4-vinylpryridine) sensor is noisy, but it does respond to the CO above 200 ppm. The polyepichlorohydrin sensor is less noisy and shows good response down to 100 ppm.

Homer, Margie L.↗