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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 19 records
All sourcesNASA NTRSDOE OSTI
DOE OSTI2022

Standard Operating Protocol for Ion-Exchange Capacity of Anion Exchange Membranes

Ion-exchange capacity (IEC) is the measure of a material’s capability to displace ions formerly incorporated within its structure. IEC is a key feature of anion-exchange membranes (AEM), as it determines the AEM’s ability to conduct the ions required to sustain the electrochemical reactions where they are utilized. As an intrinsic property, measuring the IEC accurately is essential to study AEMs and understand their performance within devices. In this method article, a facile and accurate standard operating procedure (SOP) to measure the IEC of AEMs is proposed. When compared to conventional acid-base back-titration or Mohr titration, the proposed method combines the fast reaction between silver and halide ions and the accuracy of the potentiometric titration, providing a convenient and precise protocol for researchers in the field.

42 ENGINEERING↗
DOE OSTI2025

Ether Cleavage Decreases the Ion Exchange Capacity of Anion Exchange Membranes

Anion exchange membranes (AEMs) are integral to fuel cells and water electrolysis systems but suffer from poor durability under alkaline conditions. Ether cleavage is an important failure pathway of poly(arylene ether)-based AEMs that compromises both mechanical stability and ion transport. While this degradation pathway is often studied in terms of polymer fragmentation, the role of newly formed hydrophilic groups has been largely overlooked. Here, we show that polymer scission leads to reduced mechanical rigidity, while the introduction of hydrophilic groups partially mitigates this loss. Under alkaline conditions, phenoxide groups formed during ether cleavage neutralize the polymer cations, leading to a previously unreported loss of ion exchange capacity (IEC). This IEC loss mechanism exacerbates the reduction in ionic conductivity, emphasizing the severity of ether cleavage as a degradation pathway. Recognizing that ether cleavage introduces significant chemical changes beyond polymer fragmentation provides critical insights into its interplay with other degradation mechanisms, such as the direct reduction of cationic sites by E2 and S N 2, and provides molecular-level interpretations for the concurrent effects of polymer scission and increased hydrophilicity on membrane performance.

crystal cleavage↗
NASA NTRS2005

High Temperature Thermosetting Polyimide Nanocomposites Prepared with Reduced Charge Organoclay

The naturally occurring sodium and calcium cations found in bentonite clay galleries were exchanged with lithium cations. Following the cation exchange, a series of reduced charge clays were prepared by heat treatment of the lithium bentonite at 130 C, 150 C, or 170 C. Inductively coupled plasma (ICP) analysis showed that heating the lithium clay at elevated temperatures reduced its cation exchange capacity. Ion exchange of heat-treated clays with either a protonated alkyl amine or a protonated aromatic diamine resulted in decreasing amounts of the organic modifier incorporated into the lithium clay. The level of silicate dispersion in a thermosetting polyimide matrix was dependent upon the temperature of Li-clay heat treatment as well as the organic modification. In general, clays treated at 150 C or 170 C, and exchanged with protonated octadcylamine or protonated 2,2'-dimethlybenzidine (DMBZ) showed a higher degree of dispersion than clays treated at 130 C, or exchanged with protonated dodecylamine. Dynamic mechanical analysis showed little change in the storage modulus or T(sub g) of the nanocomposites compared to the base resin. However, long term isothermal aging of the samples showed a significant decrease in the resin oxidative weight loss. Nanocomposite samples aged in air for 1000 hours at 288 C showed of to a decrease in weight loss compared to that of the base resin. This again was dependent on the temperature at which the Li-clay was heated and the choice of organic modification.

Campbell, Sandi↗
DOE OSTI2020

Understanding Multi-Ion Transport Mechanisms in Bipolar Membranes

Bipolar membranes (BPMs) have the potential to become critical components in electrochemical devices for a variety of electrolysis and electrosynthesis applications. Because they can operate under large pH gradients, BPMs enable favorable environments for electrocatalysis at the individual electrodes. Critical to the implementation of BPMs in these devices is understanding the kinetics of water dissociation that occurs within the BPM as well as the co- and counter-ion crossover through the BPM, which both present significant obstacles to developing efficient and stable BPM-electrolyzers. In this study, a continuum model of multi-ion transport in a BPM is developed and fit to experimental data. Specifically, concentration profiles are determined for all ionic species, and the importance of a water-dissociation catalyst is demonstrated. The model describes internal concentration polarization and co- and counter-ion crossover in BPMs, determining the mode of transport for ions within the BPM and revealing the significance of salt-ion crossover when operated with pH gradients relevant to electrolysis and electrosynthesis. Lastly, a sensitivity analysis reveals that the performance and lifetime of BPMs can be improved substantially by using of thinner dissociation catalysts, managing water transport, modulating the thickness of the individual layers in the BPM to control salt-ion crossover, and increasing the ion-exchange capacity of the ion-exchange layers in order to amplify the water-dissociation kinetics at the interface.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2025

Assessing the Long-Term Stability of Anion Exchange Membranes for Electrochemical CO 2 Reduction

Materials and cell components used in CO 2 electrolysis have largely been adapted from technologies initially developed for water electrolysis and fuel cells. However, electrochemical CO 2 reduction introduces distinct material challenges due to the unique chemical environment in this process. Here, in this study, we conducted ex-situ 1000 h stability tests on commonly used anion exchange membranes, exposing them exclusively to electrolytes and organic molecules used or produced during CO 2 electrolysis, at concentrations relevant to and compatible with postseparation processes. Notably, 15% w/w n-propanol and 5 M acetic acid caused complete dissolution or partial disintegration of the membranes unless cross-linking was present and remained stable throughout the test. When the membranes stayed physically intact, most of them exhibited excellent chemical stability in alkaline medium containing alcohols or formic acid, which was confirmed by vibrational spectroscopy and ion exchange capacity measurements. However, exposure to alcohol-and acid-containing solutions led to a substantial increase in swelling and water uptake, with potential implications for mechanical stability, ion/product crossover, and compression management of adjacent components. The potential effects of CO 2 electroreduction products on membrane stability, their subsequent impact on electrolyzer performance, and mitigation strategies are discussed.

CO2RR↗
NASA NTRS1975

Improved polyelectrolyte for ion exchange fibers

Technique increases ion exchange capacity of hollow-fiber-substrate ion exchange resins. Procedure increases number of quaternary sites on polyquaternary copolymer by 15 to 35 percent.

Rembaum, A.↗
DOE OSTI2021

Ionomer Optimization for Water Uptake and Swelling in Anion Exchange Membrane Electrolyzer: Hydrogen Evolution Electrode

Green hydrogen produced through anion exchange membrane water electrolysis is a promising, low-cost chemical storage solution for intermittent renewable energy sources. Low-temperature electrolysis using anion exchange membranes (AEM) combines the benefits of established water electrolysis technologies based on alkaline electrolysis and proton exchange membrane electrolysis. The anion conductive ionomers (ACI) used in the AEM electrolyzer (AEMEL) electrodes has been investigated. The ACI serves two primary purposes: (i) facilitate hydroxide conduction between the catalyst and bulk electrolyte and (ii) bind the catalyst to the porous transport layer and membrane. High ion exchange capacity (IEC) ACIs are desired, however, high IEC can cause excessive water uptake (WU) and detrimental ACI swelling. Proper water management is a key factor in obtaining maximum performance in AEM-based devices. In this study, a series of poly(norbornene)-based ACIs were synthesized and deployed in hydrogen evolving AEMEL cathode electrodes. A balance between ionic conductivity, WU and ionomer swelling was achieved in the ACI by varying the IEC and degree of polymer cross-linking. It was found that higher IEC ACIs with light crosslinking are preferred in the HER electrode. Furthermore, such a configuration fine-tuned the WU and ionomer swelling to achieve optimum cell performance and reduce cell operating voltages.

08 HYDROGEN↗
DOE OSTI2025

Uptake and binding of La 3+ and Cr 3+ ions by alkali metal substituted alpha-zirconium phosphate

The conversion of alpha-zirconium phosphate, Zr(HPO 4 ) 2 ·H 2 O, to the K-, Rb-, and Cs-phases and the subsequent ion exchange behavior of these alkali metal phases, A-ZrP, with La 3+ and Cr 3+ have been investigated. The conversion to the A-ZrP phases was achieved by reaction with metal chloride, metal hydroxide solution, and confirmed through various techniques, including X-ray powder diffraction, thermogravimetry analysis, IR spectroscopy, scanning and transmission electron microscopy, and X-ray photoelectron spectroscopy. The effect of material hydration, which increased the interlayer distance, was also examined. The ion exchange behavior of the A-ZrP showed strong affinity for both La 3+ , a representative for trivalent lanthanide metals, and Cr 3+ , a representative for the trivalent transition metals, with a rapid, near quantitative removal of the M 3+ ions at a pH of 3 when the ion concentration was ≤25% of the ion exchange capacity of the materials. Additionally, the ion affinity was shown to be pH and concentration-dependent, decreasing with a decrease in pH or an increase in ion concentration. Lastly, the binding strength of La- and Cr-loaded ZrP materials was examined through a series of leaching experiments in a carbonate buffer, phosphate buffer, HEPES buffer, and a series of EDTA solutions at various concentrations. No observable leaching occurred in the carbonate buffer, phosphate buffer, HEPES buffer, or when the EDTA concentration was below 0.1 mM. These results highlight the potential for the A-ZrP materials to provide a platform for trivalent transition metal and trivalent lanthanide radionuclide capture for various applications.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2023

LTE-P-7 IEC AEM SOP

A procedure for measuring the ion exchange capacity (IEC) of an anion exchange membrane (AEM). This is done via a titration method (automated or manual).

08 HYDROGEN↗
DOE OSTI2025

Anion exchange membrane test protocol validation

This study presents the validation of protocols for measuring ion exchange capacity (IEC) and alkaline stability of anion exchange membranes (AEMs) for low-temperature water electrolysis. While protocols are often tested within individual laboratories, their results across multiple laboratories with varying equipment, environmental conditions, and personnel qualification remain unverified. The validation involved Los Alamos National Laboratory (LANL), National Renewable Energy Laboratory (NREL), and University of Oregon (UO) using the same commercially available AEM to assess reproducibility and reliability of the protocols under diverse conditions. For the IEC protocol, results across laboratories were consistent within ±10% of the NMR-determined reference value. The alkaline stability protocol could pose greater challenges due to factors such as variations in sample collection timing, preservation methods, and analytical techniques, but consistent test results for percentage IEC loss were demonstrated across institutions. These results highlight the reliability and applicability of the protocols, emphasizing the importance of validation to ensure consistency in diverse research environments.

08 HYDROGEN↗
NASA NTRS1976

Ion-exchange hollow fibers

An ion-exchange hollow fiber is prepared by introducing into the wall of the fiber polymerizable liquid monomers, and polymerizing the monomers therein to form solid, insoluble, crosslinked, ion-exchange resin particles which embed in the wall of the fiber. Excess particles blocking the central passage or bore of the fiber are removed by forcing liquid through the fiber. The fibers have high ion-exchange capacity, a practical wall permeability and good mechanical strength even with very thin wall dimensions. Experimental investigation of bundles of ion-exchange hollow fibers attached to a header assembly have shown the fiber to be very efficient in removing counterions from solution.

Rembaum, A.↗
NASA NTRS1980

Ion-exchange hollow fibers

An ion-exchange hollow fiber is prepared by introducing into the wall of the fiber polymerizable liquid monomers, and polymerizing the monomers therein to form solid, insoluble, cross-linked, ion-exchange resin particles which embed in the wall of the fiber. Excess particles blocking the central passage or bore of the fiber are removed by forcing liquid through the fiber. The fibers have high ion-exchange capacity, a practical wall permeability and good mechanical strength even with very thin wall dimensions. Experimental investigation of bundles of ion-exchange hollow fibers attached to a header assembly have shown the fiber to be very efficient in removing counterions from solution.

Rembaum, Alan↗
NASA NTRS1977

Ion-exchange hollow fibers

An ion-exchange hollow fiber is prepared by introducing into the wall of the fiber polymerizable liquid monomers, and polymerizing the monomers therein to form solid, insoluble, cross-linked, ion-exchange resin particles which embed in the wall of the fiber. Excess particles blocking the central passage or bore of the fiber are removed by forcing liquid through the fiber. The fibers have high ion-exchange capacity, a practical wall permeability and good mechanical strength even with very thin wall dimensions. Experimental investigation of bundles of ion-exchange hollow fibers attached to a header assembly have shown the fiber to be very efficient in removing counterions from solution.

Rembaum, Alan↗
NASA NTRS1978

Cationic vinyl pyridine copolymers and products thereof

Quaternized, cross-linked, insoluble copolymers of unsubstituted and substituted vinyl pyridines and a dihalo organic compound are spontaneously formed at ambient temperature on mixing the two monomers in bulk, in solution or in suspension. The amount of cross-linking may be varied according to the composition and reaction conditions. The polymer product exhibits ion exchange capacity and undergoes a reversible color change from black at a pH above 7 to yellow at a pH below 7. The polymer may be formed in the presence of preformed polymers, substrates such as porous or impervious particles or films to deposit an ion exchange film in situ or on the surface of the substrate. The coated or resin impregnated substrate may be utilized for separation of anionic species from aqueous solution.

Rembaum, Alan↗
DOE OSTI2023

LTE-P-3 IEC PEM SOP

A procedure for measuring the ion exchange capacity (IEC) of a proton exchange membrane (PEM).

08 HYDROGEN↗