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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

Cambered Bipyridyl Ligand with Extended Aryl System Enables Electrochemical Reduction of Carbon Dioxide and Bicarbonate by Mn(bpy)(CO) 3 Br-type Catalyst Immobilized on Carbon Nanotubes

Heterogeneous materials containing molecular catalytic sites show promise for electrocatalytic reduction of CO 2 to energy-enriched carbon products. Interactions between the catalyst and the heterogeneous support increasingly are recognized as important in governing product selectivity and rate. Recent work on Mn(R-bpy)(CO) 3 Br type catalysts immobilized on multiwalled carbon nanotubes (MWCNT) demonstrated control of electrocatalytic behavior with steric modification of the molecular catalyst. Phenyl groups installed in the 4,4' positions of the bipyridine ligand (ph-bpy) maximized performance through π–π interactions with the MWCNT support. Herein we report the outcome of extending the ligand π system with Mn(nap-bpy)(CO) 3 Br (nap-bpy = 4,4'-di(naphthalen-1-yl)-2,2'-bipyridine) and Mn(pyr-bpy)(CO) 3 Br (pyr-bpy = 4,4'-di(pyren-1-yl)-2,2'-bipyridine) immobilized on MWCNT. We demonstrate exceptional electrocatalysis with Mn(nap-bpy)(CO) 3 Br/MWCNT (FE CO > 92%; J CO = 16.5 mA/cm 2 ) and find that this catalyst electrochemically reduces bicarbonate in the absence of deliberately added CO 2 at a remarkable overall selectivity of >80% for carbon products (FE HCOO – = 52% and FE CO = 29%). We show diminishing returns to simply adding aromatic character to the bipyridyl ligand with Mn(pyr-bpy)(CO) 3 Br/MWCNT and observe a unique cambering of the Mn(nap-bpy)(CO) 3 Br bipyridyl ligand that we believe enables selective catalysis. Mechanistic studies were carried out on Mn(nap-bpy)(CO) 3 Br/MWCNT using a novel thin-film infrared spectroelectrochemical (IR-SEC) technique. These experiments observe the immobilized Mn(nap-bpy)(CO) 3 Br undergo single electron reduction to a Mn-centered radical that binds CO 2 in a reduction-coupled process.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Photoelectrocatalytic reduction of CO 2 to formate using immobilized molecular manganese catalysts on oxidized porous silicon

The reduction of carbon dioxide (CO 2 ) to formate using molecular catalysts immobilized on high surface area porous silicon is described. Manganese complexes of the type ( R bpy)Mn(CO) 3 Br (bpy = 2,2′-bipyridine) were prepared with silatrane groups on the bpy ligand for attachment to oxide-coated porous silicon (SiO x -porSi). SiO x -porSi wafers were formed by heating hydrogen-terminated p-type porous silicon wafers under air, and the manganese complexes were immobilized on SiO x -porSi by heating at 80°C. The resulting hybrid photoelectrodes are photoelectrocatalysts for CO 2 reduction in acetonitrile containing 2.0 M triethylamine and 2.0 M isopropanol, yielding formate with high selectivity (>96%) and current density (∼0.6 mA/cm 2 ), excellent reproducibility, and a photovoltage of 280 mV at −1.75 V (versus ferrocenium/ferrocene) under 1 sun illumination. Here, the applied potential is close to the equilibrium potential for CO 2 reduction to formate. This work presents rare examples of immobilized molecular catalysts for CO 2 reduction to formate and the first on semiconducting silicon.

13 HYDRO ENERGY↗

Characterizing Density and Spatial Distribution of Trap States in Ta 3 N 5 Thin Films for Rational Defect Passivation

Tantalum nitride (Ta 3 N 5 ) has gained significant attention as a potential photoanode material, yet it has been challenged by material quality issues. Defect-induced trap states are detrimental to the performance of any semiconductor material. Beyond influencing the performance of Ta 3 N 5 films, defects can also accelerate the degradation in water during desired electrochemical applications. Defect passivation has provided an enormous boost to the development of many semiconductor materials but is currently in its infancy for Ta 3 N 5 . This is in part due to a lack of experimental understanding regarding the spatial and energetic distribution of trap states throughout Ta 3 N 5 thin films. Here, we employ drive-level capacitance profiling (DLCP) to experimentally resolve the spatial and energetic distribution of trap states throughout Ta 3 N 5 thin films. The density of deeper energetic traps is found to reach ∼2.5 to 6 × 10 22 cm –3 at the interfaces of neat Ta 3 N 5 thin films, over an order of magnitude greater than the bulk. In addition to the spatial profile of deep trap states, we report neat Ta 3 N 5 thin films to be highly n-type in nature, owning a free carrier density of ∼9.74 × 10 17 cm –3 . This information, coupled with the present understanding of native oxide layers on Ta 3 N 5 , has facilitated the rational design of a targeted passivation strategy that simultaneously provides a means for catalyst immobilization. Loading catalyst via silatrane moieties suppresses the density of defects at the surface of Ta 3 N 5 thin films by two orders of magnitude, while also reducing the free carrier density of films by over one order of magnitude, effectively dedoping the films to ∼2.40 × 10 16 cm –3 . The surface passivation of Ta 3 N 5 films translates to suppressed defect-induced trapping and recombination of photoexcited carriers, as determined through absorption, photoluminescence, and transient photovoltage. Here, this illustrates how developing a deeper understanding of the distribution and influence of defects in Ta 3 N 5 thin films has the potential to guide future works and ultimately accelerate the integration and development of high-performance Ta 3 N 5 thin film devices.

defect passivation↗

Durable Fuel Cell MEA through Immobilization of Catalyst Particle and Membrane Chemical Stabilizer

For hydrogen-based fuel cell electric vehicle to be cost competitive with the incumbent diesel-powered internal combustion engine heavy-duty vehicle, the total cost of ownership of the truck must be decreased via both capital cost and the operating cost (H 2 fuel expense) reduction. This puts the emphasis on the decrease of fuel cell stack cost via use of low platinum catalyst material usage to decrease capital cost, high H 2 fuel efficiency and high stack durability to decrease the operating cost. US DOE has set a target of ≤ 0.25 mgPt/cm 2 total loading in the membrane electrode assembly, high fuel efficiency of > 68% and a HD-combined target of ≥ 2.5 kW/gPGM after running an accelerated stress test (AST) equivalent to 30,000 hours of heavy-duty fuel cell operation.

08 HYDROGEN↗

Visible-Light-Responsive Photocatalysis: Ag-Doped TiO2 Catalyst Development and Reactor Design Testing

In recent years, the alteration of titanium dioxide to become visible-light-responsive (VLR) has been a major focus in the field of photocatalysis. Currently, bare titanium dioxide requires ultraviolet light for activation due to its band gap energy of 3.2 eV. Hg-vapor fluorescent light sources are used in photocatalytic oxidation (PCO) reactors to provide adequate levels of ultraviolet light for catalyst activation; these mercury-containing lamps, however, hinder the use of this PCO technology in a spaceflight environment due to concerns over crew Hg exposure. VLR-TiO2 would allow for use of ambient visible solar radiation or highly efficient visible wavelength LEDs, both of which would make PCO approaches more efficient, flexible, economical, and safe. Over the past three years, Kennedy Space Center has developed a VLR Ag-doped TiO2 catalyst with a band gap of 2.72 eV and promising photocatalytic activity. Catalyst immobilization techniques, including incorporation of the catalyst into a sorbent material, were examined. Extensive modeling of a reactor test bed mimicking air duct work with throughput similar to that seen on the International Space Station was completed to determine optimal reactor design. A bench-scale reactor with the novel catalyst and high-efficiency blue LEDs was challenged with several common volatile organic compounds (VOCs) found in ISS cabin air to evaluate the system's ability to perform high-throughput trace contaminant removal. The ultimate goal for this testing was to determine if the unit would be useful in pre-heat exchanger operations to lessen condensed VOCs in recovered water thus lowering the burden of VOC removal for water purification systems.

Photocatalysis↗

Mechanistic Insights into C–H Borylation of Arenes with Organoiridium Catalysts Embedded in a Microporous Metal–Organic Framework

Organometallic iridium catalysts can be used in conjunction with bispinacolatodiboron (B 2 Pin 2 ) to effect the borylation of a variety of substrates such as arenes, alkanes, heteroarenes, and oxygenates. Recently, efforts have also focused on integrating these catalysts into porous supports, such as metal–organic frameworks (MOFs). While the mechanism of homogeneous borylation systems has been thoroughly investigated experimentally and computationally, analogous studies in MOF-supported iridium catalysts have not been conducted. In this paper, we report the mechanistic investigation of a phenanthroline-iridium catalyst immobilized in the organic linker of Universitetet i Oslo (UiO)-67 (Zr 6 O 4 (OH) 4 (BPDC) 4 (PhenDC) 2 , BPDC = biphenyl-4,4'-dicarboxylate, PhenDC = 1,10-phenanthroline-4,4'-dicarboxylate). By using benzene as a model substrate, variable time normalization analysis (VTNA) of the kinetic data suggested a rate law consistent with zero-order in B 2 Pin 2 , and first-order in arene. A primary kinetic isotope effect (KIE) in the time course of benzene-d 6 borylation also provided complementary information about the role of the arene in the rate-determining step of the reaction. Characterization by techniques such as X-ray absorption spectroscopy (XAS) confirmed the presence of Ir(III), while pair distribution function (PDF) analysis suggested structures containing an Ir–Cl bond, further substantiated by X-ray photoelectron spectroscopy (XPS). Analysis of postcatalysis materials by inductively coupled plasma–optical emission spectroscopy (ICP-OES) revealed low boron accumulation, which may indicate an absence of boron in the resting state of the catalyst. Finally, in comparing borylation of benzene and toluene, a slight selectivity for benzene is observed, which is similar to the analogous homogeneous reaction, indicating the influence of substrate sterics on reactivity.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Charge Transport in Zirconium-Based Metal–Organic Frameworks

Metal–organic frameworks (MOFs) are a class of crystalline porous materials characterized by inorganic nodes and multitopic organic linkers. Because of their molecular-scale porosity and periodic intraframework chemical functionality, MOFs are attractive scaffolds for supporting and/or organizing catalysts, photocatalysts, chemical-sensing elements, small enzymes, and numerous other functional-property-imparting, nanometer-scale objects. Notably, these objects can be installed after the synthesis of the MOF, eliminating the need for chemical and thermal compatibility of the objects with the synthesis milieu. Thus, postsynthetically functionalized MOFs can present three-dimensional arrays of high-density, yet well-separated, active sites. Depending on the application and corresponding morphological requirements, MOF materials can be prepared in thin-film form, pelletized form, isolated single-crystal form, polycrystalline powder form, mixed-matrix membrane form, or other forms. For certain applications, most obviously catalytic hydrolysis and electro- or photocatalytic water splitting, but also many others, an additional requirement is water stability. MOFs featuring hexa-zirconium(IV)-oxy nodes satisfy this requirement. For applications involving electrocatalysis, charge storage, photoelectrochemical energy conversion, and chemiresistive sensing, a further requirement is electrical conductivity, as embodied in electron or hole transport. As most MOFs, under most conditions, are electrically insulating, imparting controllable charge-transport behavior is both a chemically intriguing and chemically compelling challenge. Herein, we describe three strategies to render zirconium-based metal–organic frameworks (MOFs) tunably electrically conductive and, therefore, capable of transporting charge on the few nanometers (i.e., several molecular units) to few micrometers (i.e., typical dimensions for MOF microcrystallites) scale. The first strategy centers on redox-hopping between periodically arranged, chemically equivalent sites, essentially repetitive electron (or hole) self-exchange. Zirconium nodes are electrically insulating, but they can function as grafting sites for (a) redox-active inorganic clusters or (b) molecular redox couples. Alternatively, charge hopping based on linker redox properties can be exploited. Marcus’s theory of electron transfer has proven useful for understanding/predicting trends in redox-hopping based conductivity, most notably, in accounting for variations as great as 3000-fold depending on the direction of charge propagation through structurally anisotropic MOFs. In MOF environments, propagation of electronic charge via redox hopping is necessarily accompanied by movement of charge-compensating ions. Consequently, rates of redox hopping can depend on both the identity and concentration of ions permeating the MOF. In the context of electrocatalysis, an important goal is to transport electronic charge fast enough to match or exceed the inherent activity of MOF-based or MOF-immobilized catalysts. Bandlike electronic conductivity is the focus of an alternative strategy: one based on the introduction of molecular guests capable of forming donor–acceptor charge transfer complexes with the host framework. Theory again can be applied predictively to alter conductivity. A third strategy similarly emphasizes electronic conductivity, but it makes use of added bridges in the form of molecular oligomers or inorganic clusters that can then be linked to span the length of a MOF crystallite. For all strategies, retention of molecular-scale porosity is emphasized, as this property is key to many applications. Lastly, while our focus is on Zr-MOFs, the described approaches clearly are extendable to other MOF compositions, as has already been demonstrated, in part, in studies by others.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Continuous multimodal technologies in industrial microbiology: potential for achieving high process performance and agility

The field of industrial microbiology has great potential to tackle the most pressing challenges facing society, but today, this entails much more than classical fermentation technology followed by product upgrading. Methods are needed to confer unit-operation-level functionality and whole-system-level robustness, as well as flexibility. As examples of this concept, we focus here on methodologies often deployed at industrial scale as discrete processes—such as biological, chemical, and electrochemical unit operations—that are also capable of substantial complementarity when combined sequentially and operated continuously. A key and relatively new type of conversion step is made possible by catalyst immobilization methods at both the enzymatic and cellular level. Cases drawn from electro-fermentation for acetoin production and syngas-mediated microbial electrosynthesis of ethanol exemplify the synergy of combined operational approaches. Because modular processes can be treated as a series of reactor elements, considerable flexibility is possible. As discussed, however, not all processes are amenable to this intensification.

09 BIOMASS FUELS↗

Carboranylmethylene-substituted phosphazenes and polymers thereof

Carboranylmethylene-substituted cyclophosphazenes are described which can be thermally polymerized into carboranylmethylene-substituted phosphazene polymers. The polymers are useful as thermally stable coatings. Also, due to the characteristics of these polymers in acting as a ligand for transition metals, metalocarboranylmethylene phosphazene polymers are described which can act as immobilized catalyst systems, and are electrically conductive and superconductive.

Allcock, H. R.↗

A General Strategy to Immobilize Single‐Atom Catalysts in Metal–Organic Frameworks for Enhanced Photocatalysis

Abstract Single‐atom catalysts (SACs) are witnessing rapid development due to their high activity and selectivity toward diverse reactions. However, it remains a grand challenge in the general synthesis of SACs, particularly featuring an identical chemical microenvironment and on the same support. Herein, a universal synthetic protocol is developed to immobilize SACs in metal–organic frameworks (MOFs). Significantly, by means of SnO 2 as a mediator or adaptor, not only different single‐atom metal sites, such as Pt, Cu, and Ni, etc., can be installed, but also the MOF supports can be changed (for example, UiO‐66‐NH 2 , PCN‐222, and DUT‐67) to afford M 1 /SnO 2 /MOF architecture. Taking UiO‐66‐NH 2 as a representative, the Pt 1 /SnO 2 /MOF exhibits approximately five times higher activity toward photocatalytic H 2 production than the corresponding Pt nanoparticles (≈2.5 nm) stabilized by SnO 2 /UiO‐66‐NH 2 . Remarkably, despite featuring identical parameters in the chemical microenvironment and support in M 1 /SnO 2 /UiO‐66‐NH 2 , the Pt 1 catalyst possesses a hydrogen evolution rate of 2167 µmol g –1 h –1 , superior to the Cu 1 and Ni 1 counterparts, which is attributed to the differentiated hydrogen binding free energies, as supported by density‐functional theory (DFT) calculations. This is thought to be the first report on a universal approach toward the stabilization of SACs with identical chemical microenvironment on an identical support.

Sui, Jianfei↗

Interfacial Electrochemistry of Catalyst-Coordinated Graphene Nanoribbons

The immobilization of molecular electrocatalysts on conductive electrodes is an appealing strategy for enhancing their overall activity relative to those of analogous molecular compounds. Here, in this study, we report on the interfacial electrochemistry of self-assembled two-dimensional nanosheets of graphene nanoribbons (GNR-2DNS) and analogs containing a Rh-based hydrogen evolution reaction (HER) catalyst (RhGNR-2DNS) immobilized on conductive electrodes. Proton-coupled electron transfer (PCET) taking place at N-centers of the nanoribbons was utilized as an indirect reporter of the interfacial electric fields experienced by the monolayer nanosheet located within the electric double layer. The experimental Pourbaix diagrams were compared with a theoretical model, which derives the experimental Pourbaix slopes as a function of parameter f, a fraction of the interfacial potential drop experienced by the redox-active group. Interestingly, our study revealed that GNR-2DNS was strongly coupled to glassy carbon electrodes (f = 1), while RhGNR-2DNS was not (f = 0.15). We further investigated the HER mechanism by RhGNR-2DNS using electrochemical and X-ray absorption spectroelectrochemical methods and compared it to homogeneous molecular model compounds. RhGNR-2DNS was found to be an active HER electrocatalyst over a broader set of aqueous pH conditions than its molecular analogs. We find that the improved HER performance in the immobilized catalyst arises due to two factors. First, redox-active bipyrimidine-based ligands were shown to dramatically alter the activity of Rh sites by increasing the electron density at the active Rh center and providing RhGNR-2DNS with improved catalysis. Second, catalyst immobilization was found to prevent catalyst aggregation that was found to occur for the molecular analog in the basic pH. Overall, this study provides valuable insights into the mechanism by which catalyst immobilization can affect the overall electrocatalytic performance.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Plasma-Initiated Graft Polymerization of Acrylic Acid onto Fluorine-Doped Tin Oxide as a Platform for Immobilization of Water-Oxidation Catalysts

The discovery of new and versatile strategies for the immobilization of molecular water-oxidation catalysts (WOCs) is crucial for developing clean energy conversion devices [e.g., (photo)electrocatalytic cells for water splitting]. The traditional approach for surface attachment to transparent conductive oxides [e.g., fluorine doped tin oxide (FTO)] is via synthetic modification of the ligand architecture to incorporate functional groups such as carboxylic acids (-COOH) or phosphonates (-PO 3 H 2 ) prior to immobilization. However, challenges arising from desorption and the cumbersome derivatizations steps have limited the scope and applications of surface-bound WOCs. Herein, we report the successful immobilization of underivatized Ru(II)-based WOCs (Ru–Cat1 = [Ru(tpy) (bpy) (H 2 O)] 2+ (tpy = 2,2':6'2"–terpyridine and bpy = 2,2;-bipyridine) and Ru–Cat2 = [Ru(Mebimpy) (bpy) (H 2 O)] 2+ (Mebimpy = 2,6-bis(1-methylbenzimidazol-2-yl) pyridine)) and the Ru(II) polypyridyl chromophore Ru–C3 = [Ru(bpy) 3 ] 2+ onto a FTO plasma-grafted poly(acrylic acid) surface (PAA|FTO). Various characterization techniques such as attenuated total reflectance Fourier transform infrared spectroscopy, scanning electron microscopy, atomic force microscopy, and cyclic voltammetry measurements provide evidence for the plasma-induced grafted PAA|FTO film and immobilization. Surface stability and electrocatalytic properties of these new hybrid composite films upon cycling were investigated at different pH values. Immobilized Ru–Cat1 and Ru–Cat2 onto PAA|FTO displayed pH-dependent (RuIII/RuII) couples and onset potentials indicative of PCET (proton-coupled electron transfer) reactions. Based on cyclic voltammetry results and spectroscopic monitoring, the immobilized WOCs Ru–Cat1 and Ru–Cat2 exhibited a higher surface stability in neutral aqueous solutions relative to Ru–C3 upon electrochemical oxidation. Furthermore, we attribute the surface PCET and stability to the presence of a water ligand in the coordination sphere of immobilized Ru–Cat1 and Ru–Cat2 which can H-bond with negatively charged carboxylate groups of the cross-linked PAA brushes. Our findings demonstrate that the plasma-grafted polymeric network onto FTO offers a versatile platform to directly anchor unmodified homogeneous WOCs or chromophores for potential applications in solar-to-fuel energy conversion.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

An Intensified Electro-Catalytic Process for Production of Formic Acid from Power Plant CO 2 Emissions (Final Technical Report)

The goal of this project was to develop and test a novel electro-catalytic method for the production of high-value formic acid from coal-derived CO 2 as a strategy to offset the cost of CO 2 capture. Formic acid is currently produced from the conversion of higher-order carbon products such as methane and/or methanol. This electro-catalytic CO 2 reduction process utilizes a highly selective catalyst in a flow-through reactor design to maximize the formic acid production rate. The specific objectives of this proposed study were to; 1) produce and screen highly selective engineered CO 2 reducing catalysts capable of exclusively producing formic acid; 2) immobilize the catalyst within a flow process to continually produce formic acid and increase catalyst lifetime; and 3) assess the stability of the electrocatalyst during long-term operation. The project involved the development and testing of an engineered catalyst to selectively reduce CO 2 directly and exclusively to formic acid. After the best-performing catalyst was selected, it was immobilized and tested inside a flow-through reactor at UK CAER using realistic conditions expected from CO 2 produced during coal combustion and separated by a CO 2 capture plant.

01 COAL, LIGNITE, AND PEAT↗

Recent Advances in Immobilizing and Benchmarking Molecular Catalysts for Artificial Photosynthesis

Transition metal complexes have been widely used as catalysts or chromophores in artificial photosynthesis. Traditionally, they are employed in homogeneous settings. Despite their functional versatility and structural tunability, broad industrial applications of these catalysts are impeded by the limitations of homogeneous catalysis such as poor catalyst recyclability, solvent constraints (mostly organic solvents), and catalyst durability. Over the past few decades, researchers have developed various methods for molecular catalyst heterogenization to overcome these limitations. Here, in this review, we summarize recent developments in heterogenization strategies, with a focus on describing methods employed in the heterogenization process and their effects on catalytic performances. Alongside the in-depth discussion of heterogenization strategies, this review aims to provide a concise overview of the key metrics associated with heterogenized systems. We hope this review will aid researchers who are new to this research field in gaining a better understanding.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Molecularly tunable heterogeneous catalysts by edge functionalization of graphitic carbons

Disclosed are surface immobilized (electro)catalysts that may be prepared by a condensation reaction that generates an aromatic unit that is robust to acid and base and elevated temperatures. Among their many desirable characteristics, the catalysts are far less prone to the bimolecular deactivation pathways commonly observed for homogeneous catalysts, and may be used in solvents with a range of polarities and dielectric strengths. The catalysts are suitable for a wide array of thermal catalytic reactions (polymerization, oxidation, hydrogenation, cross-coupling etc.) and as anodes and/or cathodes in fuel cells, electrolyzers, and in batteries and supercapacitors.

Surendranath, Yogesh↗