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NASA NTRS1993

Liquid crystalline order in mucus

Mucus plays an exceptionally wide range of important biological roles. It operates as a protective, exchange, and transport medium in the digestive, respiratory, and reproductive systems of humans and other vertebrates. Mucus is a polymer hydrogel. It is secreted as discrete packages (secretory granules) by specialized secretory cells. Mucus hydrogel is stored in a condensed state inside the secretory granules. Depending upon the architecture of their constituent macromolecules and on the composition of the solvent, polymer gels can form liquid crystalline microstructures, with orientational order being exhibited over optically resolvable distances. Individual mucin molecules consist of alternating rigid segments (heavily glycosylated; hydrophilic) and flexible segments (nonglycosylated; hydrophobic). Polymer molecules consisting of rigid units linked by flexible spacers are frequently associated with liquid crystalline behavior, which again raises the possibility that mucus could form anisotropic fluid phases. Suggestions that mucins may be self-associating in dilute solution have previously been challenged on the basis of sedimentation-equilibrium studies performed on mucus in which potential sites of association were competitively blocked with inhibitors. However, the formation of stable liquid crystalline phases does not depend on the existence of inter- or intramolecular associations; these phases can form on the basis of steric considerations alone.

NASA Discipline Number 40-20↗

DOE OSTI2022

Deconvoluting sources of failure in lithium metal batteries containing NMC and PEO-based electrolytes

Solid-state lithium metal batteries (SSLMBs) containing polyethylene oxide (PEO)-derived polymer electrolytes and high-voltage (> 4 V vs. Li/Li + ) cathode materials suffer from three sources of failure: (1) instability between the polymer electrolyte and cathode at high voltage, (2) instability of the polymer electrolyte with Li metal, and (3) poorly-designed cathodes. In this study, these three sources of failure are deconvoluted by studying Ni-rich LiNi x Mn y Co 1-x-y O 2 (NMC, x ≥ 0.6) cathodes and a gel polymer electrolyte (GPE) derived from PEO. Initial cycling data reveals that rapid capacity fade occurs regardless of whether soft short circuits form due to Li dendrites. Cyclic voltammetry scans on cells featuring a Li metal electrode, GPE, and a NMC811 electrode free of additives suggest that there are no runaway reactions between the GPE and NMC811 up to 4.5 V vs. Li/Li + . Cathode/cathode symmetric cell cycling demonstrates that Li metal reactivity is a prime source of failure, though a poorly-designed cathode leads to subpar performance. A cathode with single-crystal NMC particles was demonstrated to achieve better initial capacity and longer cycle life, indicating room for improvement in SSLMB cathode design. Therefore, the sources of failure as enumerated may be ranked as follows from most to least concerning: 2 > 3 > 1.

25 ENERGY STORAGE↗

DOE OSTI2025

Molecular Interlocking Multidimensional Modulations of Cathode‐Electrolyte Interface for Constructing High Energy Density Quasi‐Solid‐State Batteries

Gel polymers are regarded as a promising candidate electrolyte for lithium-metal quasi-solid-state batteries, primarily due to their high ionic conductivity and solid-liquid synergistic properties. However, challenges such as interfacial side reactions, limitations in Li + transport caused by interfacial issues, and leaching of transition metals from the cathode have yet to be effectively solved. Herein, a novel gel electrolyte modulation strategy based on electrostatic filler assembly is proposed to address the issues of ineffective capacity utilization and inadequate cycling stability of high-energy-density cathode materials in solid-state lithium-ion batteries. It constructs a 3D interpenetrating charge-bridge network that effectively tackles the phase-separation challenge between fillers and electrolytes at the molecular level. Meanwhile, the molecular interlocking structure effectively inhibits the electrolyte erosion. More critically, it optimizes and stabilizes the cathode-electrolyte interface film, which facilitates the conduction of Li + -ions through a size-sieving mechanism. Consequently, this strategy enables effective adaptation across diverse high-energy-density cathode materials with satisfactory capacity performance (170.4 mAh g −1 at 4.5 V/1 C for LiNi 0.6 Co 0.2 Mn 0.2 O 2 and 194.0 mAh g −1 at 4.3 V/1 C for LiNi 0.9 Co 0.08 Mn 0.02 O 2 ). In conclusion, this investigation offers a straightforward and effective reference for addressing the critical challenges of ionic transport and interface stabilization in the design of gel electrolytes.

cathode-electrolyte interface↗

DOE OSTI2020

Well-designed Crosslinked Polymer Electrolyte Enables High Ionic Conductivity and Enhanced Salt Solvation

A new facile single-step method to fabricate crosslinked polymer electrolyte membranes consisting of branched poly(ethyleneimine), (PEI) and poly(ethylene oxide), (PEO) is demonstrated. The membranes exhibit excellent ionic conductivity (1.2 × 10 –3 S cm –1 at 80 °C) with minimal addition of plasticizer (20 wt%). The amine functional group in the PEI-PEO crosslinked matrix provides Lewis basic and hydrogen bonding characteristics that facilitate the dissolution of lithium salt and enables a higher cation transport number than a PEO crosslinked matrix. The glass transition temperature, degree of crystallinity, and room temperature storage modulus increases with decreasing crosslink density and increasing ratio of free amines. The resultant ionic conductivity and mechanical strength can be flexibly tailored by varying the molar ratio of free amine moieties in the crosslinked PEI-PEO matrix. This study provides an improved synthesis method, in-depth characterization, and fundamental insights on the effect of free amine moieties on the transport properties of a highly conductive gel polymer electrolyte.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2026

Interfacial and Kinetic Origins of Voltage Loss in Neutral Zinc‐Air Batteries

Rechargeable zinc-air batteries are promising candidates for grid-scale energy storage; however, their practical deployment is limited by oxygen electrocatalysis inefficiencies and interfacial instabilities, particularly outside conventional alkaline electrolytes. Here, in this work, zinc-air batteries operating under neutral electrolyte conditions using ZnCl 2 soaked KC-PAA-PAM gel polymer electrolytes and electrochemically synthesized Ni/Fe layered double hydroxide electrocatalysts is investigated. Ni/Fe-LDH is intentionally employed as an OER-biased benchmark catalyst to diagnose electrolyte and interface driven limitations rather than as a bifunctional ORR/OER solution. Full cells exhibit highly stable cycling over hundreds of hours, yet operate at substantially suppressed charge and discharge voltages relative to the thermodynamic value. Electrochemical impedance analysis shows that ohmic losses contribute only minimally to this voltage suppression. Post-mortem X-ray photoelectron spectroscopy reveals metallic zinc accumulation on the air cathode and chloride-containing species on the anode, indicating parasitic interfacial processes. Synchrotron-based soft X-ray absorption spectroscopy confirms stable Ni 2+ and Fe 3+ oxidation states during cycling, consistent with OER-biased catalytic behavior, while neutral-electrolyte oxygen evolution measurements demonstrate strong electrolyte-induced suppression of oxygen kinetics. Together, these results show that electrolyte chemistry and cathode-side parasitic processes, rather than catalyst identity alone, dominate voltage losses in neutral zinc-air batteries, providing mechanistic insight into the fundamental challenges associated with neutral electrolyte operation.

Long duration energy storage↗

DOE OSTI2020

Keratin-derived functional carbon with superior charge storage and transport for high-performance supercapacitors

In this work, we report a scalable method to synthesize hierarchically porous, hetero-atom doped activated carbon nanosheet from waste biomass-human hair, and demonstrates the use of this carbon as an ultra-high performance electrode material for supercapacitor applications. Microscopic analyses reveal that sheet size ranges from 50 to 200 nm having a thickness of 15–27 nm. As-synthesized, carbon nanosheets possess a hierarchical porous structure having a specific surface area of 1548 m 2 g -1 . Heteroatom concentration (nitrogen, oxygen, and sulfur) of around 25% is confirmed from XPS analysis. Therefore, the novel interconnected hierarchical porous nanosheets structure enables fast adsorption and transportation of ions during electrochemical processes. Also, the abundant chemically available electroactive heteroatom species in the material enhance the wettability of ions and contribute to pseudocapacitance. The electrochemical analyses through cyclic voltammetry and galvanostatic charge-discharge measurements in 6 M KOH reveal the quasi-EDLC behavior of the activated carbons due to the presence of heteroatoms. A reprensentative KOH activated carbon shows an excellent specific capacitance value of 999 F g -1 at a current density of 1 A g -1 . Furthermore, the symmetrically assembled two-electrode device also delivers a maximum energy density of 32 W h Kg -1 at a power density of 325 W Kg -1 . In addition, excellent cyclic stability of 98% capacitance retention is observed after 10,000 continuous GCD cycles even at a high current density of 5 A g -1 . Symmetric flexible supercapacitor device using KOH-PVA-K3FeCN6 as redox gel polymer electrolyte shows a synergistic specific capacitance of 145 mF cm -1 at a current density of 0.8 mA cm -1 exhibiting very less deviation in bending mode. Therefore, this waste biomass derived heteroatom doped hierarchical porous carbon nanosheets can be a promising material for cost-effective high- performance supercapacitor.

42 ENGINEERING↗

DOE OSTI2025

Composite biopolymer electrolytes for high-performance reversible zinc-air batteries

Zinc-air batteries (ZABs) are regarded as one of the most promising candidates for next-generation energy storage systems due to their inherent safety, high energy density, and low cost. In this study, we optimized the composition of gel polymer electrolytes (GPEs), which play a crucial role in enhancing ZAB reversibility due to their water retention capabilities. The GPEs are synthesized using a combination of polyacrylic acid (PAA), polyacrylamide (PAM), and biopolymer kappa-carrageenan (KC), with and without additional additives. Among these, the composite GPE containing KC, PAA, and PAM demonstrated superior ionic conductivity (6.68 mS/cm at 30 °C) and enhanced water retention compared to the PAA–PAM-based GPE. Furthermore, this composite electrolyte operates within a wider electrochemical window of −1.0 V–2.2 V. A bifunctional catalyst, nickel–iron layered double hydroxide (NiFe-LDH), is electrochemically synthesized on a modified activated carbon cloth (CC). The catalyst loading is optimized based on oxygen evolution reaction (OER) performance, showing an overpotential of 555 mV. The oxygen reduction reaction (ORR) occurred at a half-wave potential of 0.620 V, which is lower than that of Pt/C (0.852 V), indicating better catalytic activity. The KC based cell exhibit better cycling stability than PAA–PAM-based GPE. The electrochemical performance of ZAB cells is evaluated under various atmospheres: ambient air and humid conditions and temperatures. Notably, in a humid environment, the cells achieved extended cycling stability, operating for over 500 h—significantly longer than under open-air conditions. Overall, this study highlights the importance of tailored GPE design and efficient bifunctional catalysts to enhance the performance and longevity of zinc-air batteries for long-duration energy storage applications.

Catalyst↗

DOE OSTI2021

Nanocarrier-loaded block copolymer dual domain organogels

Loaded polymer gels are prevalent materials in the controlled release community and, fairly recently, have been formulated to include nanocarrier domains such as micelles and vesicles. One mechanism used to establish the solid-like characteristic of gels is block copolymer self-assembly, which can result in a system-spanning, physically-crosslinked network. Additionally, the combination of nanocarrier and crosslink domain presence offers gels with a rich nanoscale phase space capable of intricate macroscopic property tuning. The current manuscript provides an overview of nanocarrier-loaded block copolymer organogels wherein nanocarriers are reverse micelles formed by sodium dioctyl sulfosuccinate (AOT), the block copolymer is a styrenic ABA triblock copolymer, and the gel solvent is aliphatic mineral oil. This introductory overview starts by identifying the envelope in ternary phase space wherein nanocarrier-loaded block copolymer organogels form (2-49 wt% triblock copolymer and 8x10 -3 -1 wt% AOT). Next, a detailed nanostructural description of gels varying in AOT and triblock copolymer concentration is presented. The manuscript concludes with demonstration of AOT reverse micelle release and gel uniaxial tensile response for gels containing 0-1 wt% AOT and 5-40 wt% styrenic triblock copolymer.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2022

Polyanionic insertion hosts for aqueous rechargeable batteries

Safety concerns and costs of present-day lithium-ion batteries (LIBs) are prompting the development of alternate battery technologies with different types of electrolyte ( e.g. , solid-state, gel-polymer, aqueous, etc. ); notably, systems based on aqueous electrolytes have emerged as a promising alternative, especially for grid storage applications. The last decade has witnessed a considerable spike in the research carried out on aqueous batteries. However, the narrow operating voltage window of aqueous electrolytes and the structural instability of materials in aqueous media demand proper selection of cathode materials to achieve desirable energy density. Polyanionic materials can be an ideal choice as they are structurally more stable and exhibit tunable redox potentials. This class of materials is considered as a storehouse in which many materials can be realized by substituting different polyanionic subunits. Here, this review highlights some of the recent advances made in the polyanionic class of cathode materials for rechargeable aqueous batteries (Li-, Na- and Zn-ion batteries). The challenges facing the field, possible remedies to overcome them and future perspectives are also presented.

25 ENERGY STORAGE↗

DOE OSTI2020

2020 Vehicle Technology Office Annual Progress Report from Jianchao Ye

25 ENERGY STORAGE↗

DOE OSTI2021

VTO_2021_APR_LLNL_Ye

Traditional batteries are composed of two-dimensional films that are stacked and/or rolled. Thin film batteries display high power density while their thick film counterparts show good energy density, but it has proven difficult to concurrently achieve both within these planar form factors. In addition, conventional Li-ion batteries based on liquid organic electrolytes or gel polymer electrolytes have raised severe safety concerns due to the intrinsic flammable properties of the organic electrolytes. They are also not ideal for the use of high energy density metallic lithium (Li) anodes due to Li dendrite growth, or sulfur cathodes due to shuttling effects that result in fast capacity fade. There is an urgent need to develop safe, high-performance solid-state batteries (SSBs) with advanced electrolyte and separator technologies. Although in recent years a series of superionic conductors have been developed for electrolytes and separators, their performance does not satisfy demanding criteria due to large impedance from poor solid electrolyte-electrode contact and questionable electrochemical and mechanical stability. Unlike the well-established roll-to-roll fabrication of conventional Li-ion batteries, the processing of SSBs is unique due to the brittleness of solid-state electrolytes (SSEs). The commercially available or lab-developed SSE discs are usually very thick (hundreds of micrometers to millimeters) to overcome their brittle nature, which unfortunately increases the cell impedance and accounts for the majority of the overall cell weight and volume, leading to dramatically decreased power and energy densities. In this project, we will investigate 3D printing techniques to overcome safety, fabrication, mechanical, and electrochemical issues in SSBs. 3D printing builds complex structures in a layer-by-layer fashion, which allows rapid production of hierarchical architectures, gradient and multi-material structures, and multi-component assemblies. 3D printing is an emerging area that could fundamentally transform energy storage devices. For example, 3D printing can produce batteries with arbitrary form factors to fit a product’s specific volume requirements and can create interwoven electrode arrangements over a wide range of length scales to improve transport and increase power density for a given energy density. For SSBs, 3D printing may dramatically reduce the separator thickness from ~1 mm (by hydraulic pressing) to tens of micrometers or less. In addition, the interfacial contact area between the electrolyte and the electrode may be increased via 3D interdigitated designs. Hence, we expect a significant reduction of the overall cell impedance and enhancement of both energy and power densities of SSBs by harnessing an array of 3D printing technologies being developed at Lawrence Livermore National Laboratory (LLNL).

25 ENERGY STORAGE↗

DOE OSTI2021

Using Dissipative Particle Dynamics to Model Effects of Chemical Reactions Occurring within Hydrogels

Computational models that reveal the structural response of polymer gels to changing, dissolved reactive chemical species would provide useful information about dynamically evolving environments. However, it remains challenging to devise one computational approach that can capture all the interconnected chemical events and responsive structural changes involved in this multi-stage, multi-component process. Here, we augment the dissipative particle dynamics (DPD) method to simulate the reaction of a gel with diffusing, dissolved chemicals to form kinetically stable complexes, which in turn cause concentration-dependent deformation of the gel. Using this model, we also examine how the addition of new chemical stimuli and subsequent reactions cause the gel to exhibit additional concentration-dependent structural changes. Through these DPD simulations, we show that the gel forms multiple latent states (not just the “on/off”) that indicate changes in the chemical composition of the fluidic environment. Hence, the gel can actuate a range of motion within the system, not just movements corresponding to the equilibrated swollen or collapsed states. Moreover, the system can be used as a sensor, since the structure of the layer effectively indicates the presence of chemical stimuli.

36 MATERIALS SCIENCE↗

NASA NTRS1986

Viscometer for low frequency, low shear rate measurements

A computer-controlled torsion-oscillator viscometer with low 0.5 Hz frequency and very low 0.05/s shear rate is designed to precisely study shear-sensitive fluids such as microemulsions, gels, polymer solutions and melts, colloidal solutions undergoing coagulation, and liquid mixtures near critical points. The viscosities are obtained from measurements of the logarithmic decrement of an underdriven oscillator. The viscometer is found to have a resolution of 0.2 percent when used with liquid samples and a resolution of 0.4 percent when used with a dense gaseous sample. The design is compatible with submillikelvin temperature control.

Berg, R. F.↗

NASA NTRS1996

Design of intelligent mesoscale periodic array structures utilizing smart hydrogel

Mesoscale Periodic Array Structures (MPAS, also known as crystalline colloidal arrays), composed of aqueous or nonaqueous dispersions of self-assembled submicron colloidal spheres are emerging toward the development of advanced optical devices for technological applications. This is because of their unique optical diffraction properties and the ease with which these intriguing properties can be modulated experimentally. Moreover our recent advancements in this area which include 'locking' the liquid MPAS into solid or semisolid polymer matrices for greater stability with longer life span, and incorporation of CdS quantum dots and laser dyes into colloidal spheres to obtain nonlinear optical (NLO) responses further corroborate the use of MPAS in optical technology. Our long term goal is fabrication of all-optical and electro-optical devices such as spatial light modulators for optical signal processing and flat panel display devices by utilizing intelligent nonlinear periodic array structural materials. Here we show further progress in the design of novel linear MPAS which have the ability to sense and respond to an external source such as temperature. This is achieved by combining the self-assembly properties of polymer colloidal spheres and thermoshrinking properties of smart polymer gels. At selected temperatures the periodic array efficiently Bragg diffracts light and transmits most of the light at other temperatures. Hence these intelligent systems are of potential use as fixed notch filters optical switches or limiters to protect delicate optical sensors from high intensity laser radiation.

Sunkara, H. B.↗

NASA NTRS1978

Gel Permeation Chromatography of Fluoroether Polymers

A Method is described for determining the molecular weight distribution of fluorinated polymers by gel permeation chromatography. Porous silica-packed columns are used with Freon 113 as the chromatographic solvent. Fluoroether oligomers are used for column calibration in the molecular weight range of 1400 to 12000.

Korus, Roger A.↗

NASA NTRS2001

Thermal and Cycle-Life Behavior of Commercial Li-ion and Li-Polymer Cells

Accelerated and real-time LEO cycle-life test data will be presented for a range of commercial Li-ion and Li-polymer (gel type) cells indicating the ranges of performance that can be obtained, and the performance screening tests that must be done to assure long life. The data show large performance variability between cells, as well as a highly variable degradation signature during non-cycling periods within the life tests. High-resolution Dynamic Calorimetry data will be presented showing the complex series of reactions occurring within these Li cells as they are cycled. Data will also be presented for cells being tested using an Adaptive Charge Control Algorithm (ACCA) that continuously adapts itself to changes in cell performance, operation, or environment to both find and maintain the optimum recharge over life. The ACCA has been used to prevent all unneeded overcharge for Li cells, NiCd cells and NiH2 cells. While this is important for all these cell types, it is most critical for Li-ion cells, which are not designed with electrochemical tolerance for overcharge.

Zimmerman, Albert H.↗

NASA NTRS2002

PCS: The First Fluid Physics Payload on ISS

The Physics of Colloids in Space (PCS) experiment was accommodated within International Space Station (ISS) EXpedite the PRocessing of Experiments to Space Station (EXPRESS) Rack 2 and was remotely operated from early June 2001 until February 2002 from NASA Glenn Research Center's Telescience Support Center in Cleveland, Ohio and from a remote site at Harvard University in Cambridge, Massachusetts. PCS is an experiment conceived by Professor David A. Weitz of Harvard University (the Principal Investigator), focusing on the behavior of three different classes of colloid mixtures. The sophisticated light scattering instrumentation comprising PCS is capable of color imaging, and dynamic and static light scattering from 11 to 169 degrees, Bragg scattering over the range from 10 to 60 degrees, and laser light scattering at low angles from 0.3 to 6.0 degrees. The PCS instrumentation performed remarkably well, demonstrating a flexibility that enabled experiments to be performed that had not been envisioned prior to launch. While on-orbit, PCS accomplished 2400 hours of science operations, and was declared a resounding success. Each of the eight sample cells worked well and produced interesting and important results. Crystal nucleation and growth and the resulting structures of two binary colloidal crystal alloys were studied, with the long duration microgravity environment of the ISS facilitating extended studies on the growth and coarsening characteristics of the crystals. In another experiment run, the de-mixing of the colloid-polymer critical-point sample was studied as it phase-separates into two phases, one that resembles a gas and one that resembles a liquid. This process was studied over four decades of length scale, from 1 micron to 1 centimeter, behavior that cannot be observed in this sample on Earth because sedimentation would cause the colloids to fall to the bottom of the cell faster than the de-mixing process could occur. Similarly, the study of gelation and aging of another colloid-polymer sample, the colloid-polymer gel, also provided valuable information on gelation mechanisms, as did investigations on the extremely the low concentration silica and polystyrene fractal gel samples.

Doherty, M.↗

NASA NTRS2020

An Ultra-long Life, High-performance, Flexible Li-CO2Battery Based on Multifunctional Carbon Electrocatalysts

Integrating CO2 utilization and renewable energy delivery/storage, the rechargeable Li–CO2 battery has been considered as a promising candidate for next-generation secondary batteries. However, high-performance catalyst(s) for efficient formation and decomposition of the discharge product, Li2CO3, are an imperative part of a Li–CO2 battery. The development of flexible Li–CO2 batteries extends their applications into compliant and wearable devices/systems, but at the same time imposes a big challenge for battery fabrication and lifetime enhancement. In this study, a rechargeable quasi-solidus flexible Li–CO2 battery was designed and fabricated using highly active N,S-doped carbon nanotubes (N,S-doped CNTs) as the cathode catalyst, and a smart polymer gel as the flexible electrolyte. This newly-developed flexible Li–CO2 battery exhibited a capacity as high as 23560 mAh g−1 based on the catalyst mass and an ultra-long lifetime of up to 538 cycles with excellent mechanical flexibility. This work provides a platform for the design and development of high-performance flexible Li–CO2 batteries from low-cost, earth-abundant, carbon-based multifunctional cathode catalysts.

Superior stability↗