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All sources NASA NTRS DOE OSTI

NASA NTRS2004

Lithium Polymer Electrolytes and Solid State NMR

Research is being done at the Glenn Research Center (GRC) developing new kinds of batteries that do not depend on a solution. Currently, batteries use liquid electrolytes containing lithium. Problems with the liquid electrolyte are (1) solvents used can leak out of the battery, so larger, more restrictive, packages have to be made, inhibiting the diversity of application and decreasing the power density; (2) the liquid is incompatible with the lithium metal anode, so alternative, less efficient, anodes are required. The Materials Department at GRC has been working to synthesize polymer electrolytes that can replace the liquid electrolytes. The advantages are that polymer electrolytes do not have the potential to leak so they can be used for a variety of tasks, small or large, including in the space rover or in space suits. The polymers generated by Dr. Mary Ann Meador's group are in the form of rod -coil structures. The rod aspect gives the polymer structural integrity, while the coil makes it flexible. Lithium ions are used in these polymers because of their high mobility. The coils have repeating units of oxygen which stabilize the positive lithium by donating electron density. This aids in the movement of the lithium within the polymer, which contributes to higher conductivity. In addition to conductivity testing, these polymers are characterized using DSC, TGA, FTIR, and solid state NMR. Solid state NMR is used in classifying materials that are not soluble in solvents, such as polymers. The NMR spins the sample at a magic angle (54.7') allowing the significant peaks to emerge. Although solid state NMR is a helpful technique in determining bonding, the process of preparing the sample and tuning it properly are intricate jobs that require patience; especially since each run takes about six hours. The NMR allows for the advancement of polymer synthesis by showing if the expected results were achieved. Using the NMR, in addition to looking at polymers, allows for participation on a variety of other projects, including aero-gels and carbon graphite mat en als. The goals of the polymer electrolyte research are to improve the physical properties of the polymers. This includes improving conductivity, durability, and expanding the temperature range over which it is effective. Currently, good conductivity is only present at high temperatures. My goals are to experiment with different arrangements of rods and coils to achieve these desirable properties. Some of my experiments include changing the number of repeat units in the polymer, the size of the diamines, and the types of coil. Analysis of these new polymers indicates improvement in some properties, such as lower glass transition temperature; however, they are not as flexible as desired. With further research we hope to produce polymers that encompass all of these properties to a high degree.

Berkeley, Emily R.↗

NASA NTRS2007

Composite Electrolytes for Lithium Batteries: Ionic Liquids in APTES Crosslinked Polymers

Solvent free polymer electrolytes were made consisting of Li(+) and pyrrolidinium salts of trifluoromethanesulfonimide added to a series of hyperbranched poly(ethylene oxide)s (PEO). The polymers were connected by triazine linkages and crosslinked by a sol-gel process to provide mechanical strength. The connecting PEO groups were varied to help understand the effects of polymer structure on electrolyte conductivity in the presence of ionic liquids. Polymers were also made that contain poly(dimethylsiloxane) groups, which provide increased flexibility without interacting with lithium ions. When large amounts of ionic liquid are added, there is little dependence of conductivity on the polymer structure. However, when smaller amounts of ionic liquid are added, the inherent conductivity of the polymer becomes a factor. These electrolytes are more conductive than those made with high molecular weight PEO imbibed with ionic liquids at ambient temperatures, due to the amorphous nature of the polymer.

Tigelaar, Dean M.↗

NASA NTRS2005

New Aptes Cross-linked Polymers from Poly(ethylene oxide)s and Cyanuric Chloride for Lithium Batteries

A new series of polymer electrolytes for use as membranes for lithium batteries are described. Electrolytes were made by polymerization between cyanuric chloride and diamino-terminated poly(ethylene oxide)s, followed by cross-linking via a sol-gel process. Thermal analysis and lithium conductivity of freestanding polymer films were studied. The effects of several variables on conductivity were investigated, such as length of backbone PEO chain, length of branching PEO chain, extent of branching, extent of cross-linking, salt content, and salt counterion. Polymer films with the highest percentage of PEO were found to be the most conductive, with a maximum lithium conductivity of 3.9 x 10(exp -5) S/cm at 25 C. Addition of plasticizer to the dry polymers increased conductivity by an order of magnitude.

Tigelaar, Dean M.↗

NASA NTRS2009

Room-Temperature-Cured Copolymers for Lithium Battery Gel Electrolytes

Polyimide-PEO copolymers (PEO signifies polyethylene oxide) that have branched rod-coil molecular structures and that can be cured into film form at room temperature have been invented for use as gel electrolytes for lithium-ion electric-power cells. These copolymers offer an alternative to previously patented branched rod-coil polyimides that have been considered for use as polymer electrolytes and that must be cured at a temperature of 200 C. In order to obtain sufficient conductivity for lithium ions in practical applications at and below room temperature, it is necessary to imbibe such a polymer with a suitable carbonate solvent or ionic liquid, but the high-temperature cure makes it impossible to incorporate and retain such a liquid within the polymer molecular framework. By eliminating the high-temperature cure, the present invention makes it possible to incorporate the required liquid.

Meador, Mary Ann B.↗

NASA NTRS2008

Synthesis and Compatibility of Ionic Liquid Containing Rod-Coil Polyimide Gel Electrolytes with Lithium Metal Electrodes

A highly cross-linked polyimide-polyethylene oxide copolymer has been synthesized that is capable of holding large volumes of liquid component, simultaneously maintaining good dimensional stability. An amine end capped oligomer was made that was imidized in solution, followed by reaction with a triisocyanate in the presence of desired additives at ambient temperature. Polymer films are able to hold over 4 times their weight in room temperature ionic liquid RTIL or carbonate solvent. Electrolytes were studied that contained varying amounts of RTIL, lithium trifluoromethanesulfonimide LiTFSi, and alumina nanoparticles. Electrochemical stability of these electrolytes with lithium metal electrodes was studied by galvanic cycling and impedance spectroscopy. Improved cycling stability and decreased interfacial resistance were observed when increasing amounts of RTIL and LiTFSi were added. The addition of small amounts of alumina further decreased interfacial resistance by nearly an order of magnitude. During the course of the study, cycling stability increased from less than 3 to greater than 1000 h at 60 C and 0.25 mA/cm2 current density.

Tigelaar, Dean M.↗

DOE OSTI2024

Transport of penetrants in polymeric materials

Transport phenomena of chemical species in polymers underpin many applications. This mini-review discusses several key transport scenarios in polymer gels, melts and crosslinked polymer networks. Transport mechanisms of a wide variety of penetrant and polymer chemistries are discussed via activated hopping theory and cover across the rubbery, intermediate/deeply supercooled and glassy states of polymers. Moreover, we also discuss the ionic conductivity in polymer electrolytes, emphasizing the relationship between ion diffusion and the segmental relaxation of polymers and highlighting current challenges in the community. Finally, potential research directions are suggested concerning how external fields, such as mechanical force fields, active matter and self-propelling particles, affect the particle transport in polymers. This mini-review offers a general overview of motivations for studying penetrant transports in polymers and diverse mechanisms involved.

activated hopping↗

DOE OSTI2022

Review—Electrospun Inorganic Solid-State Electrolyte Fibers for Battery Applications

Inorganic solid-state electrolytes (SSEs), especially Li 7 La 3 Zr 2 O 12 (LLZO), are promising candidates for all solid-state batteries. Generally, SSEs are synthesized by solid-state reactions at high temperatures. The high temperature required to synthesize useful polymorphs (e.g., cubic phase, in the case of LLZO) increases their production cost. To lower the synthesis temperature, several approaches, including doping and crystallite size control via sol-gel processes, have been explored. Recently, electrospinning was used to synthesize the inorganic SSE fibers to control the crystallite size and lower the calcination temperature. Several publications followed that investigated the properties of fibers and demonstrated the use of these fibers in inorganic-polymer composite SSEs. This paper presents a concise discussion of electrospinning, the parameters that control fiber morphology, the synthesis of inorganic SSE fibers, the effect of sintering conditions on the fiber morphology and composition, and the recent use of these fibers in making composite SSEs and other battery applications. Additionally, most of the discussion focuses on LLZO, but this paper also discusses applications of other types of electrospun inorganic electrolyte fibers, the challenges of using these fibers, and possible future directions in this research field.

25 ENERGY STORAGE↗

DOE OSTI2023

Semi-solid electrodes with a polymer additive

Embodiments described herein relate generally to electrochemical cells having semi-solid electrodes that include a gel polymer additive such that the electrodes demonstrate longer cycle life while significantly retaining the electronic performance of the electrodes and the electrochemical cells formed therefrom. In some embodiments, a semi-solid electrode can include about 20% to about 75% by volume of an active material, about 0.5% to about 25% by volume of a conductive material, and about 20% to about 70% by volume of an electrolyte. The electrolyte further includes about 0.01% to about 1.5% by weight of a polymer additive. In some embodiments, the electrolyte can include about 0.1% to about 0.7% of the polymer additive.

Tan, Taison↗

DOE OSTI2023

Highly swollen ROMP-based gels

In this study, the leakage of organic solvent during the transportation and storage is one of the major threats to the environment. Networks/gels acting as the absorbing materials for organic solvents are the most promising solution for the organic solvent pollution. Here, we report the synthesis of highly swollen networks/gels in high yield (≥95%) via ring opening metathesis polymerization (ROMP) using Grubbs’ first generation catalyst/initiator (G1), a crosslinker (1,1'-(methylenedi-4,1-phenylene)bis-exo-7-oxanorbornenecarboximide) and monofunctional monomer/diluent (exo-N-phenyl-7-oxanorbornenecarboximide). The mesh size of the network was varied by keeping the concentration of monomer constant while changing the concentrations of crosslinker and G1 (initiator). The swelling capacity of the network in N,N-dimethylformamide (DMF) solvent increased from 41 to 53 and to 61 with the increase of theoretical mesh size (molar ratio of monomer to crosslinker) from 20 to 40 and to 60, respectively. By further increasing the mesh size from 60 to 80 there was no significant change in swelling capacities (63). Thus, the gel with the mesh size of 60 was selected for swelling capacity analysis in other polar organic solvents such as dimethyl sulfoxide (DMSO), dichloromethane (DCM), chloroform and lithium-ion battery electrolyte solution (1.0 M LiPF 6 in ethylene carbonate (EC)/diethyl carbonate (DEC) = 50/50 (v/v)). They showed the decreased swelling capacity value from 61 to 57, 40, 31 and 5, respectively. For a controlled mesh size ROMP-based gel, we observed the highest swelling capacity values to date.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Unveiling the Reactivity of Fluoropolymers with Sodium Metal: Mechanistic Insights and Battery Implications

Poly(vinylidene fluoride-co-hexafluoropropylene) (PVDF-HFP) has broad applications across various metal-ion battery systems, such as a binder for electrodes, a supporting matrix for electrolytes, and a separator material. Due to its excellent mechanical properties, PVDF-HFP has become an excellent candidate for fabricating gel and solid-state electrolytes in sodium-based batteries. However, in this study, we noticed notable side reactions occurring at the interface of PVDF-HFP membranes and Na metal. These reactions not only alter chemical compositions but also further affect the surface morphology and adhesive properties of membranes. Similar phenomena are observed in other polyfluoroalkyl-based membranes (PVDF and PTFE). Therefore, we systematically studied the reaction mechanisms between the Na metal and these polymers. The influence of different functional groups (−F, −CF 3 , −H) and their arrangement on the reaction extent has also been discussed. Finally, we concluded with the key factors driving these side reactions and provided new perspectives for designing polymers tailored for sodium-based batteries.

Interfacial side reactions↗

DOE OSTI2023

Polymer electrolytes based on protic ionic liquids with perfluorinated anions for safe lithium-ion batteries

Here, the quest for safe and high-performance polymer electrolytes in lithium-ion batteries (LIBs) has led researchers to explore protic ionic liquids (PILs) as potential candidates to be entrapped in polymer matrices. In this context, we present an investigation into solid polymeric systems based on poly(methyl methacrylate) (PMMA) as a host for PILs, featuring 1,8-diazabicyclo-[5,4,0]-undec-7-ene (DBU) cation paired with three different anions: bis(trifluoromethanesulfonyl)imide (TFSI – ), trifluoromethanesulfonate (TFO – ), and (trifluoromethanesulfonyl-nonafluorobutylsulfonyl)imide (IM14 – ). Additionally, we explore the lithium-doped IM14-gel-like system to broaden our understanding of these intriguing materials. Through comprehensive thermal analysis, solid-state NMR, and diffusion NMR techniques, we delve into the interactions and structural features of these binary and ternary polymeric systems. Our investigation reveals unique dynamics and ion interactions within the PMMA matrix, shedding light on the potential of these materials for advanced energy storage technologies. Particularly, we highlight the distinctive features of DBUH-IM14 and its specific interaction with the polymeric matrix and the lithium ions, underscoring its significance in advancing safer and more efficient energy storage devices.

25 ENERGY STORAGE↗

DOE OSTI2023

2022 American Conference on Neutron Scattering (ACNS 2022)

The 11th American Conference on Neutron Scattering (ACNS 2022) will be held on June 5-9, 2022, in Boulder, CO. The Conference will provide essential information on the breadth and depth of current neutron-related research worldwide. Hosted by the Neutron Scattering Society of America, this year’s Conference will feature a combination of invited and contributed talks, poster sessions, and tutorials. Topics of the conference are: Advances in Neutron Facilities, Instrumentation and Software: Developments in sources, instrumentation, sample environments and control software. Hard Condensed Matter: Magnetism, correlated metals, quantum/topological materials, superconductors, ferroelectrics, multiferroics, glasses, and disorder phenomena. Submissions outlining examples of neutron scattering in industrial and engineering applications involving hard condensed matter systems are also encouraged. Soft Matter: Neutron studies of soft materials and related fields including in situ and in operando studies. Polymers, surfactants, emulsions, gels, nanoparticles, colloidal suspensions and more. Submissions of computational studies or applications of machine learning beneficial to neutron scattering experiments, as well as examples of neutron scattering in industrial and engineering applications are strongly encouraged. Biology, Biophysics and Biotechnology: Neutron studies of biological and biologically relevant systems. Proteins, bio membranes, biological assemblies, natural materials, nucleic acids, drug-delivery platforms and biomedical systems. Submissions of computational studies or applications of machine learning beneficial to biological neutron scattering experiments, as well as examples of neutron scattering in applied research involving biological systems, are strongly encouraged. Materials Chemistry and Energy: Neutron-based studies of functional materials and materials for energy applications. Examples include porous materials such as metal organic frameworks (MOFs), zeolites; phosphors; novel pigments; electrolytes; catalysts; ionic conductors/cathode materials; photovoltaic materials (hybrid perovskites); thermoelectrics; magnetocalorics/electrocalorics. Structural Materials and Engineering: Neutron scattering studies of materials and engineering processes including structural materials, concrete and metals, as well as engineering processes including combustion, corrosion, additive manufacturing, and others. Neutron Physics: Fundamental physical studies of the neutron and related areas. Emerging Applications in Neutron Scattering: Machine Learning and Data Science: Advances in computing power have contributed to rapidly evolving machine learning and data science fields that can be leveraged to the benefit of the neutron scattering community. The purpose of this session is to highlight recent advances in machine learning and data science and to serve as the foundation of a parallel data and computation track highlighting computation advances and applications in neutron scattering throughout the conference.

36 MATERIALS SCIENCE↗

NASA NTRS2017

Novel Polyimide Battery Separator Imbibed with Room-Temperature Ionic Liquids

The journey to Mars will require advancements in many existing technologies, including space power and energy storage systems. According to the 2015 NASA Technology Roadmaps, energy storage is a critical technology area to develop for both terrestrial as well as future long-term space missions. Currently, batteries represent one of the major areas in need of advancement, both in terms of energy density as well as safety. Recently, concerns regarding the fire safety of commercial lithium-ion batteries have prompted efforts to produce nonflammable battery components, namely the electrolyte and separator. Commercial lithium-ion batteries utilize polyolefin separators imbibed with a lithium salt dissolved in cyclic carbonates. This separator/electrolyte combination imparts good ionic conductivities in the range of 10(exp -2) to 10(exp -3) S/cm. However, the cyclic carbonates and polyolefin separator are inherently flammable. Room-temperature ionic liquids (RTILs) appear to be a safer alternative to cyclic carbonates. They offer good ionic conductivities, similar to those observed in cyclic carbonates, but are inherently nonvolatile and nonflammable giving them a safety advantage. Many promising RTILs for battery electrolytes are not compatible with commercial polyolefin separator materials. Polyimide aerogels possess an open-porous, fibrillar network architecture which offers a high degree of porosity (typically greater than 85 porous), required for lithium ion conduction, as well as good mechanical properties. Furthermore, these materials are compatible with all tested RTILs. By creating a polyimide gel and imbibing the gel with a RTIL containing a lithium salt instead of super critically drying them to form aerogels, a nonflammable separator/electrolyte system with conductivities in the range of 1x10(exp -3) S/cm has been demonstrated.

Polyimide↗

NASA NTRS2009

NASA Tech Briefs, May 2009

Topics covered include: Valve-"Health"-Monitoring System; Microstrip Antenna for Remote Sensing of Soil Moisture and Sea Surface Salinity; Biomedical Wireless Ambulatory Crew Monitor; Wireless Avionics Packet to Support Fault Tolerance for Flight Applications; Aerobot Autonomy Architecture; Submillimeter Confocal Imaging Active Module; Traveling-Wave Maser for 32 GHz; System Synchronizes Recordings from Separated Video Cameras; Piecewise-Planar Parabolic Reflectarray Antenna; Reducing Interference in ATC Voice Communication; EOS MLS Level 1B Data Processing, Version 2.2; Auto-Generated Semantic Processing Services; Geospatial Authentication; Maneuver Automation Software; Event Driven Messaging with Role-Based Subscriptions; Estimating Relative Positions of Outer-Space Structures; Fabricating PFPE Membranes for Capillary Electrophoresis; Linear Actuator Has Long Stroke and High Resolution; Installing a Test Tap on a Metal Battery Case; Fabricating PFPE Membranes for Microfluidic Valves and Pumps; Room-Temperature-Cured Copolymers for Lithium Battery Gel Electrolytes; Catalysts for Efficient Production of Carbon Nanotubes; Amorphous Silk Fibroin Membranes for Separation of CO2; "Zero-Mass" Noninvasive Pressure Transducers; Radial-Electric-Field Piezoelectric Diaphragm Pumps; Ejector-Enhanced, Pulsed, Pressure-Gain Combustor; Suppressing Ghost Diffraction in E-Beam-Written Gratings; Target-Tracking Camera for a Metrology System; Polarimetric Imaging using Two Photoelastic Modulators; Miniature Wide-Angle Lens for Small-Pixel Electronic Camera; Modal Filters for Infrared Interferometry; Mo(3)Sb(7-x)Te(x) for Thermoelectric Power Generation; Two-Dimensional Quantum Model of a Nanotransistor; Scanning Miniature Microscopes without Lenses; Manipulating Neutral Atoms in Chip-Based Magnetic Traps; Expansion Compression Contacts for Thermoelectric Legs; Processing Electromyographic Signals to Recognize Words; Physical Principle for Generation of Randomness; DSN Beowulf Cluster-Based VLBI Correlator; Hybrid NN/SVM Computational System for Optimizing Designs; Criteria for Modeling in LES of Multicomponent Fuel Flow; Computerized Machine for Cutting Space Shuttle Thermal Tiles; Orbiting Depot and Reusable Lander for Lunar Transportation; FPGA-Based Networked Phasemeter for a Heterodyne Interferometer; Aquarius Digital Processing Unit; Three-Dimensional Optical Coherence Tomography; Benchtop Antigen Detection Technique using Nanofiltration and Fluorescent Dyes; Isolation of Precursor Cells from Waste Solid Fat Tissue; Identification of Bacteria and Determination of Biological Indicators; Further Development of Scaffolds for Regeneration of Nerves; Chemically Assisted Photocatalytic Oxidation System; Use of Atomic Oxygen for Increased Water Contact Angles of Various Polymers for Biomedical Applications; Crashworthy Seats Would Afford Superior Protection; Open-Access, Low-Magnetic-Field MRI System for Lung Research; Microfluidic Mixing Technology for a Universal Health Sensor; Microfluidic Extraction of Biomarkers using Water as Solvent; Microwell Arrays for Studying Many Individual Cells; Droplet-Based Production of Liposomes; and Identifying and Inactivating Bacterial Spores

Source record↗