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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 127 records · Page 7
All sourcesNASA NTRSDOE OSTI
DOE OSTI2020

Toward controlled functional sequencing and hierarchical structuring in imidazolium ionenes

This focused mini-review highlights recent advances related to the design and applications of imidazolium ionenes and forward-looking perspectives. Creative strategies which employ established synthetic approaches and utilize the modularity of the imidazole moiety unlock great potential for tailoring both functional and structural features arising from precise spacing of ionic groups within the polymer backbone. Here, as imidazolium ionenes draw more interest, increased sophistication of chemical modifications and material processing is occurring, with a corresponding shift toward more demanding applications. Synthetic routes for placement and sequencing of ionic content are discussed, in addition to recent approaches to control structure and self-assembly or tune behaviors of imidazolium ionenes and composites.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2020

Surface modification of ZIF ‐90 with triptycene for enhanced interfacial interaction in mixed‐matrix membranes for gas separation

Abstract Zeolite imidazole framework (ZIF‐90) nanoparticles were chemically modified by grafting triptycene moieties. The modified nanoparticles were introduced into a triptycene‐based polyimide as fillers to generate mixed matrix membranes (MMMs) for gas separation. The incorporation of “hook‐like” triptycene moieties in both dispersed and continuous phases led to intimate contact between the two phases and thus defect‐free interfacial morphology, due to the supramolecular interlocking and π–π stacking interaction between triptycene units presented in both phases. The filler/polymer solution showed shear thickening behavior due to such strong interfacial interaction. The separation performance of the prepared composite membranes was investigated as a function of filler loading and particle surface grafting density. Pure‐gas permeation results showed that the gas permeabilities increased expectedly as the filler loading increased, with stable or improved selectivities. The reduced permeability relative to pristine polyimide film is likely due to the pore blockage of ZIF‐90 upon grafting triptycene moieties on the particle surface. Reducing the grafting density of triptycene moieties led to improved permeability and selectivity suggesting good tunability of this series of new composite membranes. Overall, modification of nanofiller with hierarchical triptycene moieties offers a fundamentally new avenue for creation of composite membranes with unique properties in gas separations.

Zhang, Qinnan↗
DOE OSTI2022

In Situ Growth of Crystalline and Polymer-Incorporated Amorphous ZIFs in Polybenzimidazole Achieving Hierarchical Nanostructures for Carbon Capture

We report mixed matrix materials (MMMs) hold great potential for membrane gas separations by merging nanofillers with unique nanostructures and polymers with excellent processability. In situ growth of the nanofillers is adapted to mitigate interfacial incompatibility to avoid the selectivity loss. Surprisingly, functional polymers have not been exploited to co-grow the nanofillers for membrane applications. Herein, in situ synergistic growth of crystalline zeolite imidazole framework-8 (ZIF-8) in polybenzimidazole (PBI), creating highly porous structures with high gas permeability, is demonstrated. More importantly, PBI contains benzimidazole groups (similar to the precursor for ZIF-8, i.e., 2-methylimidazole) and induces the formation of amorphous ZIFs, enhancing interfacial compatibility and creating highly size-discriminating bottlenecks. For instance, the formation of 15 mass% ZIF-8 in PBI improves H- 2 permeability and H- 2 /CO 2 selectivity by approximate to 100% at 35 degrees C, breaking the permeability/selectivity tradeoff. This work unveils a new platform of MMMs comprising functional polymer-incorporated amorphous ZIFs with hierarchical nanostructures for various applications.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2020

2D Single-Atom Catalyst with Optimized Iron Sites Produced by Thermal Melting of Metal–Organic Frameworks for Oxygen Reduction Reaction

Zeolitic-imidazolate-frameworks-8 (ZIF-8) derivatives have recently been demonstrated as one of the most ideal precursors to prepare single-atom metal catalysts for oxygen reduction reaction (ORR). However, abundant single-atom metal sites are buried in the derived carbon nanoparticles, rendering them useless for ORR. In this work, a novel ZIF-8 "thermal melting" strategy is proposed to prepare a high specific surface area of Fe-N-doped graphene nanosheets (Fe-N/GNs) with single-atom Fe-sites on the surface which are accessible to electrolytes, optimizing their utilization and improving ORR activity. As a result, the Fe-N/GNs material exhibits excellent ORR activity with half-wave potentials of 0.903 V in alkaline media and 0.837 V in acidic media, which are comparable to commercial Pt/C catalysts.

2D↗
DOE OSTI2021

Investigations of Polymethacrylate Tribochemical Films Using X-Ray Spectroscopy and Optical Profilometry

This study investigates the elemental composition and surface morphology of solid tribochemical films formed on steel surfaces. The reversible addition-fragmentation chain transfer (RAFT) method was used to synthesize nine different metal-free polymers, which were blended into commercial base oils. The polymers were either homopolymers of dodecyl methacrylate and ethylhexyl methacrylate or were co-polymers of these monomers with six polar monomers. After tribological testing at 100 degrees C using the ball-on-flat geometry, the resulting tribochemical films were imaged using scanning electron microscopy (SEM) and optical microscopy. The resulting tribochemical films have thicknesses around 50-100 nm. Two of the films corresponding to small (P1-imidazole-containing copolymer) and large (P3-less polar homopolymer) wear were cross-sectioned using focused ion beam (FIB) and analyzed for elemental composition using energy-dispersive X-Ray (EDX) mapping. Oxygen and nitrogen enrichment was observed, consistent with the relative chemical composition of the precursor polymers. Transmission electron microscopy (TEM) evidence suggests that at the worn surface, some organic elements penetrate or are mixed into the steel substrate giving an interlocking appearance. The two samples examined with TEM showed that P1 tribofilm is diffused or mixed with the steel substrate more so than P3, suggesting a stronger affinity and contact during tribofilm formation.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2022

Revealing the dynamics of the alloying and segregation of Pt-Co nanoparticles via in-situ environmental transmission electron microscopy

Thermal treatment is a general and efficient way to synthesize intermetallic catalysts and may involve complicated physical processes. So far, the mechanisms leading to the size and composition heterogeneity, as well as the phase segregation behavior in Pt-Co nanoparticles (NPs) are still not well understood. Here, via in-situ environmental transmission electron microscopy, the formation dynamics and segregation behaviors of Pt-Co alloyed NPs during the thermal treatment were investigated. It is found that Pt-Co NPs on zeolitic imidazolate frameworks-67-derived nanocarbon (NC) are formed consecutively through both particle migration coalescence and the Ostwald ripening process. The existence of Pt NPs is found to affect the movement of Co NPs during their migration. With the help of theoretical calculations, the correlations between the composition and migration of the Pt and Co during the ripening process were uncovered. Herein, these complex alloying processes are revealed as key factors leading to the heterogeneity of the synthesized Pt-Co alloyed NPs. Under oxidation environment, the Pt-Co NPs become surface faceted gradually, which can be attributed to the oxygen facilitated relatively higher segregation rate of Co from the (111) surface. This work advances the fundamental understanding of design, synthesis, and durability of the Pt-based nanocatalysts.

36 MATERIALS SCIENCE↗
DOE OSTI2021

ZIF-8 derived carbon materials with multifunctional selective adsorption abilities

We report a family of carbon materials (denoted SFZ8C) prepared from templated carbonization of zeolitic imidazolate framework-8 (ZIF-8) in NaCl-ZnCl 2 eutectic salt. The hard-templating effect of the salt is utilized to sustain the framework and maximize the porosity during carbonization. In addition to rich surface nitrogen and oxygen species, SFZ8Cs have large specific surface area. These combined features give rise to excellent adsorption properties for light hydrocarbon gases. SFZ8Cs have both C 2 H 2 /CO 2 selective and C 3 /C 2 selective adsorption, as well as the ability to selectively remove impurities from methane. Particularly noteworthy is the excellent C 3 /C 2 selective adsorption performance by SFZ8C-900. Its propane/ethane selectivity (7.68) is on par with the best value (7.72) reported so far, yet SFZ8C-900 excels in propane uptake capacity. Here, the multifunctional properties together with the ease for the mass production make SFZ8Cs promising for a number of important applications.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Diversifying hierarchical ionic assembly by docking cations to anions as salt bridges

Here, we expand the diversity of building blocks available for ionic assembly by introducing tertiary (3°) ammonium cations into anion complexes. We use proton transfer between 3° amines and organo-phosphoric acids to generate H-bonding cations (R 3 NH + ) and anions (RHPO 4 – ) that co-assemble with cyanostar macrocycles into assemblies with 2:2:2 stoichiometry. At the heart is a supramolecular dimer where phosphate anions form salt bridges by H-bonding with cations. Unlike conventional 4° ammonium cations, 3,000 commercial amines provide diversity for high-throughput screening of 72 combinations (9 nitrogen bases and 8 acids), producing 13 privileged partners for quantitative assembly. Yields depend on the solvent and sterics of salt bridge formation. Ten more nitrogen bases connect to fluorophores (pyrene), photocatalysts (quinoline), drugs (Cipralex, Zytiga), and ionic liquids (imidazole). The synthesis and examination of 82 new salts exemplify how acid-base chemistry can open a pipeline to a diversity of building blocks for exploring hierarchical ionic assembly.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2024

Synergistic Ru Co atomic pair with enhanced activity toward levulinic acid hydrogenation

Development of efficient metal-based catalysts is of great importance for levulinic acid (LA) hydrogenation to γ-valerolactone (GVL). The widely employed Ru-based catalysts are advantageous for H 2 dissociation, however, the steric hindrance for large Ru particles hampers their coordination to C=O moiety in LA, and thereby decreasing the activity. Herein, we report a Ru 1 Co 1 -N-C double single-atom catalyst (DSAC) with synergistic Ru and Co atomic pairs for LA hydrogenation into GVL. The Ru and Co doped zeolitic imidazole frameworks (RuCo-doped ZIF-8) precursor was rationally designed ((Ru+Co)/(Zn+Ru+Co) = 2 at.%), where the Zn node spatially isolates Ru and Co species, expanding the adjacent Ru-Co distance and facilitating the formation of the Ru-Co atomic pair upon pyrolysis, with each atom coordinated with three nitrogen atoms (N 3 -Ru 1 Co 1 -N 3 ). The Ru 1 Co 1 -N-C catalyst exhibits outstanding catalytic activity, with a turnover frequency (TOF) of 1980 h –1 , surpassing previously reported Ru-based catalysts. Experimental investigation and density functional theory (DFT) calculations reveal that the electron-rich Ru induced by less electronegative Co facilitates H 2 dissociation, while atomic Ru in dual-atomic pairs promotes C=O activation, Ru and Co atomic pairs synergistically enhancing LA conversion to GVL. In conclusion, this research will shed light on the precise control of active sites at atomic scale, and also provides a new concept for designing high-performance Ru-based catalysts towards LA hydrogenation to GVL.

Double single-atom catalysts↗
DOE OSTI2023

A bioinspired cobalt catalyst based on a tripodal imidazole/pyridine platform capable of water reduction and oxidation

The prototypical drug carrier [Co II (L 1 )Cl]PF 6 (1), where L 1 is a tripodal amine bound to pyridine and methyl-imidazoles, had its electrocatalytic water splitting activity studied under different pH conditions. This species contains a high-spin 3d 7 Co II metal center, and is capable of generating both H 2 from water reduction and O 2 from water oxidation. Turnover numbers reach 390 after 3 h for water reduction. Initial water oxidation activity is molecular, with TONs of 71 at pH 7 and 103 at pH 11.5. The results reveal that species 1 can undergo several redox transformations, including reduction to the 3d 8 Co I species that precedes a LS 3d 6 hydride for water reduction, as well as nominal Co IV $=$O and Co III -OOH species required for water oxidation. Finally, post-catalytic analyses confirm the molecular nature of reduction and support initial molecular activity for oxidation.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2024

Influence of metal organic framework glasses on thermoelectric properties of AgSb 0.96 Zn 0.04 Te 2 alloy

In recent years, a significant number of chalcogenides-based thermoelectric (TE) materials have been investigated theoretically and experimentally. However, the efficiency of TE materials is often limited by physical and chemical stability issues. Therefore, it is crucial to identify additive materials that can reduce thermal conductivity and improve the efficiency of crystalline TE materials. One well-known approach to lower thermal conductivity is introducing porosity into the material structure, which helps scatter phonon energy. Metal-organic framework (MOF) crystalline materials, known for their porosity and physical and chemical stability, offer unique advantages in TE applications. In this study, we investigate the influence of 20 weight% amorphous Zeolitic Imidazolate Framework (ZIF)-62 to p-type AgSb 0.96 Zn 0.04 Te 2 (ASTZ), a well-known TE material. We synthesized composites, ASTZ, ASTZ-Zn, and ASTZ-Co, by sintering ASTZ with amorphous ZIF-62(Zn) and ZIF-62(Co) respectively. The addition of amorphous ZIF-62(Zn) leads to a significant enhancement in the Seebeck coefficient of ASTZ increasing from 151 µV/K to 229 µV/K at 586K. Moreover, the thermal conductivity of the ASTZ TE materials drops drastically from 0.491 Wm -1 K -1 to around 0.22 Wm -1 K -1 at 623K with the addition of either amorphous ZIF-62(Zn) or ZIF-62(Co). Remarkably, ASTZ containing amorphous ZIF-62(Zn) achieves a maximum thermoelectric figure of merit (zT max ) of approximately 0.078 at 573K, surpassing any MOF-based thermoelectric material reported to date. In conclusion, these findings highlight the potential of amorphous ZIF-62 as an effective additive for enhancing the properties of thermoelectric materials.

36 MATERIALS SCIENCE↗
DOE OSTI2020

A pair of metal organic framework (MOF)-derived oxygen reduction reaction (ORR) and oxygen evolution reaction (OER) catalysts for zinc-air batteries

Metal organic frameworks (MOFs) are amazing precursors for the development of functional catalysts due to their ability of being modified both structurally and in terms of composition. Here this work presents a pair of MOF - derived oxygen reduction reaction (ORR) and oxygen evolution reaction (OER) catalysts for the advancement of zinc-air batteries. Zeolitic imidazolate frameworks (ZIF) are known as ideal materials to create doped carbons. Combining with a sacrificial tellurium template, we have developed a “pseudo-carbon nanotube” with a ZIF-8 that is doped with a mixture of zinc, cobalt, and iron. The resulting mixed-metal doped porous carbon nanotubes (CoFeZn@pCNT) show excellent catalytic activity for ORR with a half-way ORR potential (E 1/2 ) of 0.87 V vs. RHE (reverse hydrogen electrode). Iridium-based catalysts are known as the best option for OER so far, but it is not viable for practical applications due to cost restrictions. Previous research into alternative catalysts has focused on metal oxides with first-row transition metals. Metal sulfides provide superior conductivity compared to metal oxides and are a new frontier in the search for affordable, active, and stable OER catalysts. By combining cobalt, iron, and nickel into a MOF structure (ZIF-67), followed by a sulfurization process, a MOF-derived mixed-metal sulfide catalyst (FeCoNi–S@ZIF) has been developed in this study. The resulting catalysts show an onset OER potential of 1.65 V vs. RHE at 10 mA cm -2 and exhibit remarkable stability for the operation of zinc-air batteries.

25 ENERGY STORAGE↗
DOE OSTI2024

Support size regulated ruthenium-sulfoacid-nitrogen sites intensify cellulose hydrogenolysis to 1,2-propylene glycol

Rational design of metal-acid-base multifunctional catalysts for upgrading cellulose to 1,2-propylene glycol (1,2-PG) is of great significance for building a sustainable world. However, it is time-consuming and tedious to regulate metal-acid-base sites to balance major reactions to render a high 1,2-PG yield. We herein report support size simultaneously regulated ruthenium-sulfoacid-nitrogen (Ru–SO 3 H–N) sites for cellulose hydrogenolysis to high yield 1,2-PG. Originated from the depolymerization and reassembly of zinc-1,3,5-benzenetricarboxylic acid (ZnBTC) fiber with zeolitic imidazolate framework (ZIF-8) in water, 2-methylimidazole infiltrated nanorod (ZnBTC(mIM)) with a varied aspect ratio was fabricated by varying the feed ratio of ZIF-8/ZnBTC. Upon being pyrolyzed, sulfonated and impregnated with Ru ions, the supported sites were tailored in terms of Ru single-atom/nanocluster ratio, SO 3 H acidity and N basicity. Further, the elaborately fabricated catalyst delivers 32.3% yield of 1,2-PG, corresponding to a high productivity of 67.71 mol h -1 g Ru -1 and a large turnover number of 34193, two and three orders of magnitude higher than those by using other Ru-containing catalytic systems for cellulose hydrogenolysis. The excellent performance can be attributed to optimized electronic and molecular structure of Ru–SO 3 H–N sites that can improve rate-determining cellulose hydrolysis/fructose hydrogenolysis, pivotal glucose isomerization with others to proceed at a matched rate. This study opens a new avenue to facilely tailor the metal-acid-base sites by rational design of size controlled supporting matrix.

1,2-Propylene glycol↗
DOE OSTI2023

Insights into the substrate specificity, structure, and dynamics of plant histidinol-phosphate aminotransferase (HISN6)

Histidinol-phosphate aminotransferase is the sixth protein (hence HISN6) in the histidine biosynthetic pathway in plants. HISN6 is a pyridoxal 5'-phosphate (PLP)-dependent enzyme that catalyzes the reversible conversion of imidazole acetol phosphate into L-histidinol phosphate (HOLP). Here, we show that plant HISN6 enzymes are closely related to the orthologs from Chloroflexota. The studied example, HISN6 from Medicago truncatula (MtHISN6), exhibits a surprisingly high affinity for HOLP, which is much higher than reported for bacterial homologs. Moreover, unlike the latter, MtHISN6 does not transaminate phenylalanine. High-resolution crystal structures of MtHISN6 in the open and closed states, as well as the complex with HOLP and the apo structure without PLP, bring new insights into the enzyme dynamics, pointing at a particular role of a string-like fragment that oscillates near the active site and participates in the HOLP binding. When MtHISN6 is compared to bacterial orthologs with known structures, significant differences arise in or near the string region. The high affinity of MtHISN6 appears linked to the particularly tight active site cavity. Finally, a virtual screening against a library of over 1.3 mln compounds revealed three sites in the MtHISN6 structure with the potential to bind small molecules. Such compounds could be developed into herbicides inhibiting plant HISN6 enzymes absent in animals, which makes them a potential target for weed control agents.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2024

Advanced Functional Materials ZnO@ZIF-8 Heterostructures for Neuromorphic Synaptic Devices

Metal-Organic Frameworks have shown great promise for memristive synaptic devices because of their adaptable electrical properties and inherent porosity, which help in efficient ion transport and storage of functional molecules. However, the limited conductivity and sensitivity to moisture associated with most MOF materials hinder their use in electronic applications. In this study, MOFs derived from metabolites have been synthesized, using ZnO as a self-sacrificial metallic source to grow Zeolitic Imidazolate Framework-8 (ZIF-8), forming ZnO@ZIF-8 heteronanostructures for neuromorphic applications. These hybrids ZnO@ZIF-8 act as promising candidates for advanced electronic applications. Through systematic investigations, including a comparison of ZnO@ZIF-8 bilayer devices with ZnO single-layer counterparts, a significant discovery emerged. The bilayer synaptic devices outperformed their single layer counterparts in electrical characteristics, as evidenced by Current-Voltage curve analysis and Long-Term Potentiation/Long Term Depression (LTP/LTD) measurements. Additionally, the ZnO layer thickness (10, 30, 50 nm) has been emphasized and the effects of annealing at 300°C in a vacuum were carefully studied for Neuromorphic Synaptic Devices. Remarkably, the 10 nm ZnO layer exhibited the lowest set voltage and a consistent On/Off ratio. This work marks a significant advancement in understanding bilayer synaptic devices, highlighting the crucial role of ZIF-8 in shaping the future of neuromorphic systems

Kolleboyina, Jayaramulu↗
DOE OSTI2022

PGM-Free Oxygen-Reduction Catalyst Development for Proton-Exchange Membrane Fuel Cells: Challenges, Solutions, and Promises

Proton-exchange membrane fuel cells (PEMFCs) are efficient and clean hydrogen energy technologies for transportation and stationary applications. Highly active and durable low-cost cathode catalysts for the oxygen-reduction reaction (ORR) under challenging acidic environments are desperately needed to address the cost and durability issues of PEMFCs. The most promising platinum group metal (PGM)-free catalysts for the ORR in acidic media are atomically dispersed and nitrogen-coordinated metal site catalysts denoted as M–N–C, M = Fe, Co, or Mn. Due to significant efforts in the past few decades, these catalysts have demonstrated much-improved ORR activity and promising initial fuel cell performance approaching traditional Pt/C catalysts. However, the insufficient long-term stability (up to 5000 h) under PEMFC operation represents a primary technical barrier to making current PGM-free catalysts less viable yet in PEMFCs. In this Account, we highlight recent advances in synthesizing efficient PGM-free catalysts for the ORR in PEMFCs, emphasizing effective strategies to improve mass and intrinsic activity and the possible degradation mechanisms. In particular, a chemical doping method based on the zeolitic imidazolate framework (ZIF)-8 represents the key to developing efficient M–N–C catalysts containing atomically dispersed and nitrogen-coordinated single metal active sites (i.e., MN 4 ). The newly acquired understanding of the formation mechanism of MN 4 active sites during the thermal activation and its correlation to catalytic properties guide the rational catalyst design rather than relying on current trial-and-error approaches. Considerable efforts have further been invested in increasing the active site density and enhancing intrinsic activity by regulating carbon-phase structures and the local coordination environment. Furthermore, these highly active catalysts usually suffer from significant activity loss during the ORR. Therefore, breaking the activity–stability trade-off is the key to simultaneously achieving activity and stability in one catalyst, which is discussed on the basis of our recent successes in regulating local carbon structures surrounding active single metal sites. Significant research efforts toward understanding the degradation mechanisms and improving the lifetime of PGM-free catalysts are still crucial for viable applications in the future. Novel electrode designing strategies are needed to translate the PGM-free catalysts’ ORR activity to solid-state electrolyte-based membrane electrode assemblies (MEAs) with robust three-phase (i.e., gas–liquid–solid) interfaces for efficient charge and mass transports for performance improvement. On the basis of our effort at the University at Buffalo supported by ElectroCat Consortium associated with U.S. DOE’s Hydrogen and Fuel Cell Technologies Office, we provide a perspective on PGM-free cathode catalysts concerning remaining bottlenecks and future opportunities, aiming to inspire the community in both mechanistic understanding and technological development.

08 HYDROGEN↗
DOE OSTI2023

In Situ Synchrotron X-ray Scattering Investigation of Cathodic ZIF-8 Deposition on Graphite Using 3D-Printed Cells

Electrochemical approaches provide unique means to fabricate thin films of metal organic frameworks (MOFs). However, the kinetics of electrochemical MOF deposition has not been quantitatively investigated so far. In this study, we report the first in situ measurements of electrochemical MOF growth using transmission synchrotron X-ray scattering. Electrochemical cells based on poly(lactic acid) with two windows were fabricated using fused-deposition modelling. Here, the resulting 3D-printed cells, the surface of which was coated with paraffin wax to prevent solvent percolation through the polymer material, were used to monitor the cathodic growth of zeolitic imidazolate framework-8 (ZIF-8) on graphite in a methanol solution containing ZnCl 2 and 2-methylimidazole (Hmim) at different cathodic potentials. The resulting time-resolved X-ray diffraction data showed a gradual increase in crystal size with negligible changes in crystal orientation during the cathodic ZIF-8 deposition. More importantly, the time-resolved data provided a means to quantitatively assess the kinetics of the cathodic ZIF-8 growth using the Gualtieri model, revealing that the cathodic potential and Hmim concentration affected crystal growth kinetics, but not nucleation kinetics. These ZIF-8 samples exhibited changes in X-ray diffraction pattern after being washed with methanol and dried in air, indicating that in situ measurements are essential to investigate mechanisms behind MOF electrodeposition.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗