Search NASA⌕ Search

SEARCH · Search NASA

Results for “Metal oxide nanoparticles”

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.

Quote a phrase for an exact phrase match. Source license links do not imply unrestricted reuse.

At least 325 records · Page 18

Engineering Ultrathin Alloy Shell in Au@AuPd Core-Shell Nanoparticles for Efficient Plasmon-Driven Photocatalysis

Bimetallic core-shell nanoparticles (NPs) possessing a synergetic coupling of plasmonic and catalytic metals have emerged as promising prototypes for efficient plasmon-driven photocatalysis. Here, Au@AuPd core-shell NPs composed of Au core NP and ultrathin AuPd shell are introduced to acquire improved light utilization efficiency in photocatalytic selective oxidation. With systematical control of the composition of the ultrathin alloy shell, it reveals that the Au@AuPd core-shell NPs with 10 at% Pd (in the single-atom alloy regime) is an effective nanostructure capable of maximizing the quantum yield of plasmon-induced light absorption and optimizing the surface electronic structure for catalytic reactions. This controlled system provides new insights into shell engineering for enhancing photocatalytic performance via the regulation of energy funneling processes in core-shell nanocatalysts.

36 MATERIALS SCIENCE↗

Lithium-excess cathode material and co-precipitation formation method

A lithium-excess cathode material according to Li1+xNiaMnbCocModO2−y (0<x<0.3, 0≤a≤1, 0≤b≤1, 0≤c≤1, 0≤d≤0.2, 0≤y≤0.25) in the form of secondary spherical microparticles formed from primary spherical nanoparticles. The primary nanoparticles can in the range of ˜130 nm to 170 nm and the secondary in the range of ˜2-3 μm. A method of formation includes mixing a carbonates or hydroxides solution into a mixed solution of transition metal (M) ions with predetermined stoichiometry under stirring, and aging resulting transition metal carbonates or hydroxides at a predetermined temperature for period of time to produce primary nanoparticles of a predetermined size. A gas-solid interface reaction to uniformly creating oxygen vacancies without affecting structural integrity of Li-excess layered oxides is also provided.

Meng, Ying Shirley↗

Unifying principles for catalytic hydrotreating processes (Final Technical Report)

This project builds on the hypothesis that the hydrotreating processes for the removal of oxygen and sulfur are fundamentally similar at the atomic-scale and existing knowledge from the treatment of petroleum derived feedstock can be leveraged for the design of novel catalysts for the upgrade of bio-oil. We tested this hypothesis by comparing computed potential energy diagrams for hydrodesulfurization (HDS) of thiophene over MoS 2 with hydrodeoxygenation (HDO) of furan over MoO 3 and concluded that certain aspects, such as catalyst promotion with transition metals, are valid strategies for both reactions. On the other hand, we also noticed significant differences in the mechanism for hydrogen (H 2 ) activation, which requires sites with metallic character. While MoS 2 is known to have metallic edge states that can catalyze H 2 dissociation, this elementary step is prohibitively slow on defect-free oxides. Only in the presence of vacancies or by creating metal/oxide interfaces can efficient H 2 activation sites during HDO be formed. The need for bifunctional catalyst when it comes to efficient and selective HDO or dehydrogenation reactions was further corroborated in joint experimental and theoretical studies of the Guerbet reaction for the coupling of biomass derived oxygenates over PdCu alloys, nitrate reduction over In-promoted Pd nanoparticles, and ethylene dehydroaromatization over Ga-exchanged ZSM-5 zeolites. All of these catalytic systems have in common that catalytic sites with distinct functional requirements are needed to create a working catalyst. Detailed computational studies were carried out for HDO of m -cresol and phenol on Ru-modified TiO 2 surfaces, which allowed us to attribute catalytic activity to the metal/oxide interface. A surprising finding was that heterolytic cleavage of the H-H bond across the Ru/TiO 2 interface was critically important, despite lower barriers for homolytic H 2 activation on Ru metal. The explanation lies in the high barriers for hydrogen spillover from Ru to TiO 2 , which becomes unnecessary in the heterolytic activation pathway. Moreover, we also reported that proton transfer steps between metal and oxide sites are mediated by weakly adsorbed surface water. During attempts to develop and validate a kinetic Monte Carlo (kMC) model for HDO reactions at the Ru/TiO 2 interface, it became clear that lateral interactions are paramount to describe realistic surface chemistry and without these interactions, the reduction and hydroxylation behavior from our simulations was inconsistent with reported experiments. To assess the importance of lateral interactions in popular computational catalyst design strategies relying on the identification of reactivity descriptors, which can be used along with Brønsted–Evans–Polanyi (BEP) and scaling relations as input to a microkinetic model (MKM) to make predictions for activity or selectivity trends, we compared predicted trends with those obtained from descriptor-based kMC models. We critically evaluated the benefits of kMC over MKM in terms of trend predictions and computational cost when using only a small set of input parameters. After confirming that in the absence of lateral interactions the kMC and MKM approaches yield identical trends and mechanistic information, we observed substantial differences between the two kinetic models when lateral interactions were introduced. The mean-field implementation applies coverage corrections directly to the descriptors, causing an artificial overprediction of the activity of strongly binding metals. In contrast, the cluster expansion in kMC implementation can differentiate among the highly active metals but it is very sensitive to the set of included interaction parameters. Considering that computational screening relies on a minimal set of descriptors, for which MKM makes reasonable trend predictions at a ca. three orders of magnitude lower computational cost than kMC, we concluded that the MKM approach does provide an overall better entry point for computational catalyst design. Overall, this project has led to 11 peer-reviewed publications, and their scientific is impact is well illustrated by their combined 702 citations.

08 HYDROGEN↗

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

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

Tigelaar, Dean M.↗

Surface engineering of Pt nanocatalysts with transition metal oleates for selective catalysis: a case study on the hydrogenation of α,β-unsaturated aldehydes

Selective and active catalysts enable effective use of feedstocks, reduced energy consumption and waste generation. Tuning the electronic structure of heterogeneous metal nanocatalysts via their surface modifications is a promising strategy to design highly selective and active catalysts for the synthesis of harder to make and more cost-efficient products. Here, we introduce transition metal oleates as a new class of ligands to engineer the catalytically active and very selective surface in organic solvents. Using citral hydrogenation and 5 nm Pt NPs as a model reaction and model catalytic system, respectively, we show that surface engineering of Pt nanocatalysts with metal oleates allows synthesis of desired partially hydrogenated product (geraniol) with ∼90% conversion with selectivity over 93%. We demonstrate that the selective synthesis of the unsaturated alcohols catalyzed by Pt NPs modified by adsorption of the transition metal salts cannot be explained by the widely accepted mechanism of preferred coordination of C$=$O groups by Lewis acids (e.g. partially oxidized transition surface metals). Our results indicate that C$=$O groups prefer to bind to negatively charged surfaces. We propose the explanation on how the adsorption of transition metal oleates can result in the increased electron density at the surface of Pt nanoparticles. Our study not only provides reliable solutions to selective hydrogenation but opens a new possibility of using metal oleates for the electronic ligand effect.

Kwon, Soon Gu [Argonne National Laboratory (ANL), ↗

Controlling Pinhole Radius and Areal Density in a-Si/SiOx Using Metal-Assisted Chemical Etching

Polysilicon on silicon oxide (poly-Si/SiOx) passivating contacts with predominant charge-carrier transport via pinholes are currently prepared via a>1000 degrees C thermal step to induce oxide break-up. Herein, we develop the precursor of a pinhole-enabled poly-Si/SiOx contact utilizing room temperature metal-assisted chemical etching (MACE) to form pinholes in the SiOx. The pinholes were created via electroless Ag nanoparticle (Ag NP) deposition followed by the MACE of intrinsic amorphous hydrogenated silicon (a-Si:H) on SiOx, creating isolated mesopores through the film stack. By varying the MACE etching solution (HF:H2O2) concentration, we were able to vary the pinhole areal density over four orders of magnitude (104-107 cm-2). We observed the Ostwald ripening of the Ag NP to enable control over the pinhole radii. Our work demonstrates proof-of-concept for a-Si:H/SiOx with mesopores across the film stack, which may serve as precursor for the development of poly-Si/SiOx passivating contacts of both polarities.

MATERIALS SCIENCE,SOLAR ENERGY↗

Facile Synthesis of a Broad Range of Colloidal Nanocrystals by Membrane-Mediated pH Gradient under Ambient Conditions

We report a simple synthesis process for a wide variety of ultrasmall nanocrystals. Simply immersing a dialysis bag containing an aqueous solution of a metal salt mixed with citric acid in a NaOH solution reservoir for 10 min, nanocrystals measuring only a few nanometers in size are formed inside the dialysis bag. We demonstrated the synthesis of ultrasmall nanocrystals of Co, Ni, Cu, Ag, Au, Pd, Cu 2 O, FeO, and CeO 2 , and found that the gradual change in pH caused by the diffusion of OH – ions through the dialysis membrane played an essential role in the formation of these nanocrystals. This method can be readily adapted for almost all transition metal elements, providing researchers in the fields of catalysis and nanomedicine an easy access to a wide range of ultrasmall metal and oxide nanocrystals.

36 MATERIALS SCIENCE↗

Infrared reflection absorption spectroscopy and temperature-programmed desorption studies of CO adsorption on Ni/CeO 2 (111) thin films: The role of the ceria support

Ceria-supported Ni has shown unique catalytic activity due to unique properties of small Ni particles and strong metal-support interaction. Identification of adsorption sites and understanding the chemical interaction over Ni-ceria at the fundamental level provide crucial insights into the reaction pathways of complex catalytic processes. In this study, to probe the surface sites, the adsorption of CO was carried out with model Ni/ceria systems consisting of Ni nanoparticles vapor-deposited on well-ordered CeO x (111) (1.5 < x < 2) thin films using infrared reflection absorption spectroscopy (IRRAS) and temperature-programmed desorption (TPD) under ultrahigh vacuum (UHV) conditions. Fully oxidized CeO 2 (111) (Ce 4+ ) and partially reduced CeO 1.75 (111) (Ce 4+ /Ce 3+ ) thin films were grown on Ru(0001) to examine the role of the ceria support. Additionally, Ni with low coverages (e.g., 0.2 ML) grows forming small two-dimensional particles on ceria at 300 K, which develop into three-dimensional clusters after heating to 700 K. In the absence of Ni, CO adsorption at 1 mTorr at 100 K shows distinct IR bands at 2158 cm -1 on CeO 2 and 2165 cm -1 on CeO 1.75 . Bridging and atop IR bands associated with CO adsorption over metallic Ni were observed on the Ni-CeO 1.75 surface at 300 K under UHV conditions. CO adsorption over Ni 0 was also observed over as-deposited Ni on CeO 2 . However, a new IR band at 2146 cm -1 due to CO adsorption over Ni 2+ species was detected at 100 K over the annealed Ni particles on CeO 2 . CO IRRAS data suggest the oxidation of Ni to Ni 2+ on CeO 2 and the formation of predominant Ni 2+ species with heating, which is further confirmed with CO TPD data and previous x-ray photoelectron spectroscopy results.

36 MATERIALS SCIENCE↗

Ultrathin alumina passivation for improved photoelectrochemical water oxidation catalysis of tin oxide sensitized by a phosphonate-functionalized perylene diimide first without, and then with, CoOy

Previously, a photoanode composed of nanostructured SnO 2 coated with the perylene diimide dye N,N'-bis(phosphonomethyl)-3,4,9,10-perylenediimide (PMPDI) plus photoelectrochemically deposited cobalt oxide (CoO y ) was shown to photoelectrochemically oxidize water at 31 ± 7% faradaic efficiency. A non-ideal part of that prior system is that the addition of the known CoO y water oxidation catalyst (WOC) resulted in a reduction of the total photocurrent rather than the anticipated increase, due to an increase in charge-carrier recombination. Herein, we show deposition of an ultrathin alumina overlayer applied by atomic layer deposition (ALD) on the SnO 2 /PMPDI photoanode can improve the photoactivity and catalytic activity of the system; the addition a ca. 1 nm-thick AlO x layer deposited on a 4000 nm (i.e., 4 micron) thick mesoporous anode system can and does have a positive, 2.5-fold improvement in the steady-state photocurrent with 29 ± 9% faradaic efficiency vs. the control anode without alumina passivation by reducing charge-carrier recombination. Moreover, ALD-deposited AlO x layer does help support the understanding of the “anti-catalysis” of co-depositing a CoO y WOC on the SnO 2 /PMPDI DS-PECs—specifically the picture of direct CoO y –SnO 2 contact-mediated recombination—but that AlO x layer was unable to improve the photocurrent in a net SnO 2 /PMPDI/AlO x (/CoO y ) system. We attribute the lack of a performance enhancement by CoOy WOC to incomplete coverage of each SnO 2 nanoparticle by the AlO x . Overall, we find the addition of an optimized ultrathin AlOx layer (0.6 nm thick; deposited at 85 °C) improves the SnO 2 /PMPDI/AlO x system's photoactivity by a factor of up to ca. 3-fold with reduced recombination. These results document that metal-oxide passivation by low-temperature ALD can be an effective strategy for improving the water oxidation performance of even nanostructured dye sensitized-photoelectrochemical cell.

36 MATERIALS SCIENCE↗

Efficient Intermolecular Energy Exchange and Soft-ionization of Water at Nanoplatelet Interfaces

X-ray, energetic photon and electron irradiation can ionize and electronically excite target atoms and molecules. These excitations undergo complicated relaxation and energy transfer processes that ultimately determine the manifold of system responses to the deposited excess energy. In weakly bound gas- and solution-phase samples, intermolecular Coulomb decay (ICD) and electron-transfer mediated decay (ETMD) can occur with neighboring atoms or molecules leading to efficient transfer of the excess energy to the surroundings. In ionic solids such as metal-oxides, intra- and inter-atomic Auger decay produces localized final states that lead to lattice damage and typically removal of cations from the substrate. The relative importance of Auger stimulated damage (ASD) versus ICD and ETMD in micro-solvated nanoparticle interfaces is not known. Though ASD is generally expected, essentially no lattice damage and very efficient ICD and ETMD resulting from ionization and electronic excitation of micro-solvated boehmite (AlOOH) nanoplatelets has been observed. Efficient energy transfer and soft ionization of interfacial molecules is likely a general phenomenon at gas-oxyhydroxide nanoparticle interfaces where the density of states of the ionized chemisorbed species significantly overlap the core hole states of the solid.

Jones, Brant M.↗

Stable Co-valorization of Carbon Dioxide and Methane via Dynamic Reconstruction of a Metal Oxide Solid Solution Catalyst

Dry reforming of methane (DRM) is a process that converts two greenhouse gases (methane and carbon dioxide) into syngas, a mixture of H 2 and CO, that can lead to a variety of value-added chemicals. Owing to its endothermic nature, high reaction temperatures up to 800 °C are typically required and the grand challenge lies in developing robust catalysts without sintering and coking-induced deactivation during the long-term on-stream operation. Towards this aim, herein, a robust complex oxide-supported NiCu alloy catalyst was generated in situ during DRM. By leveraging the configurational stability of a solid oxide solution precursor, tightly anchored NiCu bimetallic nanoparticles were in situ exsoluted and acted as the active sites in DRM. The as-afforded catalyst exhibited stable performance for DRM due to the ability to repel coke off the surface as the reaction proceeds. Kinetic experiments along with top surface characterization detail the reconstruction behavior of the solid oxide solution under DRM reaction conditions. In conclusion, the fundamental insights from this work provide guidance on generating resistant and flexible catalysts via in situ active sites formation from easily synthesized metal oxide solid solutions.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

CO 2 hydrogenation over rhodium cluster catalyst nucleated within a manganese oxide framework

Rhodium-based manganese oxide frameworks were explored as a prototype for carbon dioxide reactive capture and conversion. Three-dimensional frameworks of MnOx were utilized as support structures to isolate Rh metal centers. V, Na, and Zn were introduced as counterions to stabilize the structure and for their beneficial effect as promoters. Here, with this multicomponent catalyst, Rh active centers with MnOxs and varied counterions, we were able to selectively tune the catalytic performance of the material via the choice of counterion and structure of the host material. With cryptomelane-type tunnel manganese oxides octahedral molecular sieve (OMS2), we found that Rh-V-OMS2 was highly stable even after 48 hours on stream with a reaction rate of around 1.5x10 -4 mol CO 2 /g Rh /s, surpassing the net reactivity of other initially more active combinations. Furthermore, during CO 2 hydrogenation, in situ XAFS showed that single Rh atoms nucleated into nanoparticles/ sub-nanometer clusters with a coordination number of 5.5 or less. Our finding of the correlation between the reaction rate and particle size offers the potential for enhanced control over the reaction rate by tuning particle size. Our activity study with control experiments demonstrates that the activities of the catalysts are proved due to the unique metal support interaction offered by the Rh-X-MnO.

10 SYNTHETIC FUELS↗

Oxide dispersion strengthened 304 L stainless steel produced by ink jetting and laser powder bed fusion

This paper discusses the fundamentals of a novel hybrid method to synthesize oxide dispersion strengthened (ODS) 304 L stainless steel (SS) alloy using a modified laser powder bed fusion (LPBF) machine. Previously, ODS metal matrix composites have been produced by LPBF via ball-milling, which is expensive to scale. Here, we selectively dope yttria nanoparticles into a SS matrix by jetting a precursor chemistry onto the SS substrate prior to laser conversion and consolidation. Here, the new alloy shows good room temperature mechanical properties. Microstructures are studied using electron microscopy, energy dispersive spectroscopy and electron backscatter diffraction.

36 MATERIALS SCIENCE↗

Methods for Intercalating and Exfoliating Hexagonal Boron Nitride

Methods that facilitate exfoliation of hexagonal boron nitride (hBN), exfoliated hBN, and associated intermediate products are disclosed. Such a method can include the acts of mixing a sample of hBN with an activation agent (e.g., NaF, etc.) and a selected set of chemicals (e.g., a metal chloride) and intercalating the set of chemicals into the hBN to obtain intercalated hBN. Additionally, such a method can include the acts of hydrating the set of chemicals (i.e., the intercalates), and converting the set of chemicals to a set of oxide nanoparticles when exfoliating the intercalated hBN. The exfoliated hBN can be washed (e.g., with HCl, etc.) to remove remaining nanoparticles.

Hung, Ching-cheh↗

Strategies for regeneration of Pt-alloy catalysts supported on silica for propane dehydrogenation

Catalyst stability, resistance to deactivation, and regeneration remain a challenge for high temperature reaction processes. For Pt alloys used in propane dehydrogenation (PDH), the primary pathways of catalyst deactivation include coke formation and metal nanoparticle sintering over time. Recent work shows that silica-supported catalysts provide excellent selectivity for this reaction, but the regenerability of silica-supported catalysts has not been established. In this work, we study a series of Pt alloys, including PtMn, PtZn, and PtSn, for the PDH reaction at 550 °C and 600 °C, and we subject the catalysts to regeneration over multiple cycles. While oxidation in air restores the reactivity completely with minimal catalyst sintering, it is surprising to find that these catalysts can also be regenerated in pure hydrogen. Here we explore the types of coke formed on these catalysts using in situ temperature programmed oxidation (TPO). Two types of coke are found: one on the metallic NP surface, and a second on the silica support. Our work shows that treatment in hydrogen causes redistribution of the coke between the metal and support, which can restore most catalytic activity lost during a reaction run. Finally, periodic introduction of H 2 during a reaction cycle may constitute an unexplored strategy for extending the lifetime of PDH catalysts.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Temporal Ni K-Edge X-ray Absorption Spectroscopy Study Reveals the Kinetics of the Ni Redox Behavior of the Iron-Nickel Oxide Bimetallic OER Catalyst

Operando X-ray absorption spectroscopy (XAS) can be utilized to probe the phase and structural changes of FeNiOx and similar transition metal oxide electrocatalysts during electrocatalytic reactions. However, capturing the temporal changes occurring in the operando chemistry of electrocatalysts has been little studied. Here, in this work, we successfully capture the time-resolved changes at the Ni K-edge for both the X-ray absorption near-edge structure (XANES) and extended X-ray absorption fine structure (EXAFS) regions of an aqueous phase synthesized FeNiO x bimetallic nanoparticle electrocatalyst. During a stepped voltage experiment, the temporal change in the Ni K-edge was observed as the applied voltage was stepped from 0.7 to 0.8 V versus the silver/silver chloride reference electrode, and the change observed is associated with the Ni redox transition from the 2+ to 3+/4+ oxidation state. Individual XAS spectra were obtained in 90 s, and a total of 9 scans post voltage step showed a unique transition from a hydroxide to an oxyhydroxide phase. The shift in absorption edge energy position and the changes in spectral shape for individual scans explain the typically observed broadening of the Ni K-edge XANES spectrum during time-averaged operando XAS, and a kinetic analysis revealed a first-order observed rate constant, |k obs |, of 0.00426 s –1 and a half-life (t 1/2 ) of 163 s. Multivariate curve resolution-alternating least squares analysis followed by linear combination fitting analysis for time-averaged versus time-resolved Ni K-edge changes upon voltage step show distinct differences in estimated contributions from Ni 2+ oxide/hydroxide phases. Detailed EXAFS modeling shows the phase transition from hydroxide to oxyhydroxide on top of the unchanged metallic core.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Intense cavitation-assisted electric discharge as a promising tool for water treatment

This study investigates interrelations between one-electrode Cavitation-Assisted Electric Discharge (CAED), two-electrode CAED, and recently discovered Intense CAED (I-CAED). The one-electrode CAED is a self-triggered nanosecond discharge with pulse energy in the micro-Joule range, which can be generated even by a DC voltage. I-CAED consists of a non-equilibrium part within a low-pressure cavitating region and a micro-spark traversing a liquid film. We hypothesize that CAED propagates from the high-voltage electrode as an ionization wave through bubbles of saturated vapor. Subsequently, the streamer-like discharges in the bubbles may form a continuous plasma channel. Inside the cavitating region, the plasma is strongly non-equilibrium, providing an ideal environment for generating chemically unstable species such as hydrogen peroxide (H 2 O 2 ). Plasma of I-CAED spark is characterized by high electron density and near-thermal equilibrium, emitting a continuous ultraviolet spectrum. The combination of these different discharge parts makes I-CAED in water a highly effective tool for the Advanced Oxidation Process, particularly in water disinfection. Experimentally demonstrated Electric Energy per Order value for disinfection of E. coli-contaminated water is as low as 0.135 ± 0.035 kWh/m 3 /order. Estimates show that the implementation of “dry electrodes” configuration reduces the erosion rate of the electrode material by at least one order of magnitude. Spectral analysis reveals that the continuum emission generated by I-CAED in proximity to metal electrodes deviates from the spectra of discharges spatially decoupled from the electrodes. We assume that this spectral divergence is attributable to blackbody-like emission originating from metallic nanoparticles form during the electrode's erosion process.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗