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At least 1,657 records · Page 92
All sourcesNASA NTRSDOE OSTI
DOE OSTI2020

A Review of Microwave-Assisted Synthesis-Based Approaches to Reduce Pd-Content in Catalysts

This review article focuses on the latest advances in the synthesis of inorganic nano-catalysts using microwave heating, which has progressed significantly since its initial implementation in the mid-1980s. Over the years, nanoparticles (NPs), which inherently offer better surface accessibility for heterogeneous catalysis, have been synthesized using a wide array of heating methods. Microwave heating is one such method and employs a unique heating mechanism that can have several benefits for catalysis. When compared to conventional form of heating which relies on inter-layer mixing via convection, microwave heating operates through the chemical polarity in the target chemicals leading to an “inside-out” mode of heating. This heating mechanism is more targeted and therefore results in rapid synthesis of catalytically active NPs. Platinum group metals (PGM) have classically been the focus of nano-catalysis; however, recent efforts have also applied non-PGM group metals with the goals of lower costs, and ideally, improved catalytic reactivity and durability. This is especially of interest with respect to Pd because of its current historically high cost. Investigations into these new materials have primarily focused on new/improved synthetic methods and catalytic compositions, but it is important to note that these approaches must also be economic and scalable to attain practical relevance. With this overarching goal in mind, this review summarizes notable recent findings with a focus on Pd-dilution and microwave heating in a chronological fashion.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Promoted Ru/PrOx Catalysts for Mild Ammonia Synthesis

Ammonia synthesis is one of the most important chemical reactions. Due to thermodynamic restrictions and the reaction requirements of the current commercial iron catalysts, it is also one of the worst reactions for carbon dioxide emissions and energy usage. Ruthenium-based catalysts can substantially improve the environmental impact as they operate at lower pressures and temperatures. In this work, we provide a screening of more than 40 metals as possible promoter options based on a Ru/Pr2O3 catalyst. Cesium was the best alkali promoter and was held constant for the series of double-promoted catalysts. Ten formulations outperformed the Ru-Cs/PrOx benchmark, with barium being the best second promoter studied and the most cost-effective option. Designs of experiments were utilized to optimize both the pretreatment conditions and the promoter weight loadings of the doubly promoted catalyst. As a result, optimization led to a more than five-fold increase in activity compared to the unpromoted catalyst, therefore creating the possibility for low-ruthenium ammonia synthesis catalysts to be used at scale. Further, we have explored the roles of promoters using kinetic analysis, X-ray Photoelectron Spectroscopy (XPS), and in situ infrared spectroscopy. Here, we have shown that the role of barium is to act as a hydrogen scavenger and donor, which may permit new active sites for the catalyst, and have demonstrated that the associative reaction mechanism is likely used for the unpromoted Ru/PrOx catalyst with hydrogenation of the triple bond of the dinitrogen occurring before any dinitrogen bond breakage.

Chemistry↗
DOE OSTI2024

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↗
DOE OSTI2017

Multiple Populations in NGC 1851: Abundance Variations and UV Photometric Synthesis in the Washington and HST /WFC3 Systems

The analysis of multiple populations (MPs) in globular clusters (GCs), both spectroscopically and photometrically, is key in understanding their formation and evolution. The relatively narrow Johnson U, F336W, and Stromgren and Sloan u filters have been crucial in exhibiting these MPs photometrically, but in Paper I we showed that the broader Washington C filter can more efficiently detect MPs in the test case GC NGC 1851. Additionally, In Paper I we detected a double main sequence (MS) that has not been detected in previous observations of NGC 1851. We now match this photometry to NGC 1851's published RGB abundances and find that the two RGB branches observed in C generally exhibit different abundance characteristics in a variety of elements (e.g., Ba, Na, and O) and in CN band strengths, but no single element can define the two RGB branches. However, simultaneously considering [Ba/Fe] or CN strength with either [Na/Fe], [O/Fe], or CN strength can separate the two photometric RGB branches into two distinct abundance groups. Matches of NGC 1851's published SGB and HB abundances to the Washington photometry shows consistent characterizations of the MPs, which can be defined as an O-rich/N-normal population and an O-poor/N-rich population. Photometric synthesis for both the Washington C filter and the F336W filter finds that these abundance characteristics, with appropriate variations in He, can reproduce for both filters the photometric observations in both the RGB and the MS. This photometric synthesis also confirms the throughput advantages that the C filter has in detecting MPs.

79 ASTRONOMY AND ASTROPHYSICS↗
DOE OSTI2012

A synthesis of carbon dioxide emissions from fossil-fuel combustion

This synthesis discusses the emissions of carbon dioxide from fossil-fuel combustion and cement production. While much is known about these emissions, there is still much that is unknown about the details surrounding these emissions. This synthesis explores 5 our knowledge of these emissions in terms of why there is concern about them; how they are calculated; the major global efforts on inventorying them; their global, regional, and national totals at different spatial and temporal scales; how they are distributed on global grids (i.e. maps); how they are transported in models; and the uncertainties associated with these different aspects of the emissions. The magnitude of emissions 10 from the combustion of fossil fuels has been almost continuously increasing with time since fossil fuels were first used by humans. Despite events in some nations specifically designed to reduce emissions, or which have had emissions reduction as a byproduct of other events, global total emissions continue their general increase with time. Global total fossil-fuel carbon dioxide emissions are known to within 10% uncertainty (95% 15 confidence interval). Uncertainty on individual national total fossil-fuel carbon dioxide emissions range from a few percent to more than 50 %. The information discussed in this manuscript synthesizes global, regional and national fossil-fuel carbon dioxide emissions, their distributions, their transport, and the associated uncertainties.

29 ENERGY PLANNING, POLICY, AND ECONOMY↗
NASA NTRS1965

Threshold logic - a synthesis approach.

Book on threshold logic for logical design of digital systems including threshold element synthesis by iteration, tabulation and network synthesis

NETWORK SYNTHESIS↗
NASA NTRS1990

Prebiotic synthesis of histidine

The prebiotic formation of histidine (His) has been accomplished experimentally by the reaction of erythrose with formamidine followed by a Strecker synthesis. In the first step of this reaction sequence, the formation of imidazole-4-acetaldehyde took place by the condensation of erythrose and formamidine, two compounds that are known to be formed under prebiotic conditions. In a second step, the imidazole-4-acetaldehyde was converted to His, without isolation of the reaction products by adding HCN and ammonia to the reaction mixture. LC, HPLC, thermospray liquid chromatography-mass spectrometry, and tandem mass spectrometry were used to identify the product, which was obtained in a yield of 3.5% based on the ratio of His/erythrose. This is a new chemical synthesis of one of the basic amino acids which had not been synthesized prebiotically until now.

Non-NASA Center↗
NASA NTRS2016

VLTI-AMBER Velocity-Resolved Aperture-Synthesis Imaging of Eta Carinae with a Spectral Resolution of 12 000: Studies of the Primary Star Wind and Innermost Wind-Wind Collision Zone

The mass loss from massive stars is not understood well. Eta Carinae is a unique object for studying the massive stellar wind during the luminous blue variable phase. It is also an eccentric binary with a period of 5.54 yr. The nature of both stars is uncertain, although we know from X-ray studies that there is a wind-wind collision whose properties change with orbital phase. Aims. We want to investigate the structure and kinematics of Car's primary star wind and wind-wind collision zone with a high spatial resolution of approx.6 mas (approx.14 au) and high spectral resolution of R = 12 000. Methods. Observations of Car were carried out with the ESO Very Large Telescope Interferometer (VLTI) and the AMBER instrument between approximately five and seven months before the August 2014 periastron passage. Velocity-resolved aperture-synthesis images were reconstructed from the spectrally dispersed interferograms. Interferometric studies can provide information on the binary orbit, the primary wind, and the wind collision. Results. We present velocity-resolved aperture-synthesis images reconstructed in more than 100 di erent spectral channels distributed across the Br(gamma) 2.166 micron emission line. The intensity distribution of the images strongly depends on wavelength. At wavelengths corresponding to radial velocities of approximately -140 to -376 km/s measured relative to line center, the intensity distribution has a fan-shaped structure. At the velocity of -277 km/s, the position angle of the symmetry axis of the fan is 126. The fan-shaped structure extends approximately 8.0 mas (approx.18:8 au) to the southeast and 5.8 mas (approx.13:6 au) to the northwest, measured along the symmetry axis at the 16% intensity contour. The shape of the intensity distributions suggests that the obtained images are the first direct images of the innermost wind-wind collision zone. Therefore, the observations provide velocity-dependent image structures that can be used to test three-dimensional hydrodynamical, radiative transfer models of the massive interacting winds of Eta Car.

Velocity-resolved aperture-synthesis images↗
NASA NTRS2020

A Deformed Geometry Synthesis Technique for Determining Stacking and Cryogenically Induced Preloads for the Space Launch System

The Space Launch System (SLS) stacking and Core Stage (CS) fueling induce significant preloads that contribute to the liftoff pad separation “twang”. To accurately capture this, an approach is required that can replicate the physics of all SLS physical stacking steps, CS cryogenic shrinkage, associated geometric nonlinearities, and the transient behavior and decay of the preloads with changing boundary conditions as the vehicle separates from the pad. The Deformed Geometry Synthesis (DGS) approach presented here satisfies the above requirements. DGS determines induced preloads by modeling components in their deformed geometry states and then enforcing compatibility by closing the resulting “deadbands”. DGS seamlessly integrates into the multibody modal synthesis framework and does not require the use of artificial external loads to enforce preloads or post-processing steps to remove their influence. Since DGS iterates to solve for the deformed state inclusive of geometric nonlinearities, running linearized parametrics to exercise different potential orientations of ball jointed struts that connect the CS to Boosters for cryo-shrinkage analyses is entirely avoided. Relative to the transient behavior and decay of stacking and cryo-induced preloads with SLS liftoff pad separation, this is an area of considerable interest to the SLS program. To capture this in the most accurate way possible, DGS algorithms are designed to work with Henkel-Mar nonlinear pad separation algorithms which operate on the separating longitudinal and lateral degrees of freedom (DoFs) between the vehicle and the pad. As the separating DoFs release, in whatever manner as dictated by the interface geometries, interface loads and interface flexibilities as well as the external loading on the vehicle, the subject preloads generate a complex twang/decay time-trace as dictated by the physics of the problem. This paper presents DGS numerical verification against the closed-form solution for Timoshenko’s 3 ball-jointed strut preload problem. This problem is then extended by the authors to the geometric nonlinear case where DGS is compared to the Newton-Raphson solution of the nonlinear equations. Next, DGS is utilized to solve the SLS stacking and cryogenic shrinkage coupled loads analyses. Finally, Henkel-Mar pad separation simulations are executed that isolate the impact of the induced preloads’ twang and decay characteristics.

Space Launch System↗
NASA NTRSDate not supplied

Vortex Beam Sidelobe Suppression via Bayliss Synthesis from a Rectangular Phased Array

We demonstrate the application of the Bayliss synthesis method for suppression of sidelobes in an OAM vortex beam, when generated by a commercial-of-the-shelf, rectangular phased array. The method is optimized for the current application and simulated for a 26.5 GHz signal in CST Microwave Studio. Sidelobes are notably reduced by 16.9 dB, with minimal reduction in gain and increase in beamwidth, as compared to a uniformed stimulated phased array. Further, the OAM modes are found to have greater purity that that of the uniformly stimulated array, as well as for other amplitude tapering methods. The Bayliss synthesis is then applied to a phased array in a test range, verifying the simulation results that demonstrate sidelobe suppression. These results indicate that OAM may be applied to existing phased arrays with minimal effort.

Orbital Angular Momentum (OAM)↗
NASA NTRSDate not supplied

Vortex Beam Sidelobe Suppression via Bayliss Synthesis from a Rectangular Phased Array

We demonstrate the application of the Bayliss synthesis method for suppression of sidelobes in an OAM vortex beam, when generated by a commercial-of-the-shelf, rectangular phased array. The method is optimized for the current application and simulated for a 26.5 GHz signal in CST Microwave Studio. Sidelobes are notably reduced by 16.9 dB, with minimal reduction in gain and increase in beamwidth, as compared to a uniformed stimulated phased array. Further, the OAM modes are found to have greater purity that that of the uniformly stimulated array, as well as for other amplitude tapering methods. The Bayliss synthesis is then applied to a phased array in a test range, verifying the simulation results that demonstrate sidelobe suppression. These results indicate that OAM may be applied to existing phased arrays with minimal effort.

Orbital Angular Momentum (OAM)↗
DOE OSTI2011

SYNTHESIS AND CHARACTERIZATION OF SMART FUNCTIONAL COATINGS BY CHEMICAL SOLUTION DEPOSITION METHODS

New coating technology enables the fabrication of low cost structural health monitoring (SHM) and tamper indication devices that can be employed to strengthen national and international safeguards objectives. In particular, such innovations could serve the safeguards community by improving both the timeliness of detection and confidence in verification and monitoring. This work investigates the synthesis of functional surface coatings using chemical solutions deposition methods. Chemical solution deposition has recently received attention in the materials research community due to its unique advantages such as low temperature processing, high homogeneity of final products and the ability to fabricate materials with controlled surface properties and pore structures. The synthesis of functional coatings aimed at modifying the materials conductivity and optical properties was investigated by the incorporation of transition element (e.g. Cr{sup +3}) and rare earth (e.g. Er{sup +3}) serving as dopants in a polymer or gel matrix. The structural and morphological investigation of the as-deposited films was carried out using UV/Vis and photoluminescence (PL) spectroscopy. The as deposited coating was further investigated by scanning electron microscopy and energy dispersive x-ray microscopy.

98 NUCLEAR DISARMAMENT, SAFEGUARDS, AND PHYSICAL P↗
DOE OSTI2011

Electrodeposition of Metals in Catalyst Synthesis: The Case of Platinum Monolayer Electrocatalysts

The concern about energy sources, their availability, and related environmental effects, is at an all time high. Proton Exchange Membrane Fuel Cells (PEMFCs) - with an efficiency higher than that of internal combustion engines, light weight, low operating temperature, and fast-start-up capability - are strong candidates for automotive applications. Transportation applications could be especially important in shaping up the new energy economy since they may entail a substantial decrease in the adverse environmental effects linked to the use of fossil fuels and prolong their availability. The largest portion of the cost of PEMFCs reflects the large amount of Pt needed in the cathode's catalytic layer due to the low catalytic activity of Pt for the oxygen reduction reaction (ORR). Recently, considerable advances have been made in fuel cell electrocatalysis yielding improved electrocatalysts, and increasing our understanding of the kinetics of the ORR in combination with significant advances in theoretical treatments. Some of these studies involved: (1) alloying Pt to synthesize bi-metallic catalysts, (2) core-shell nanoparticles catalysts, (3) the role of size, structure, and shape of nanoparticles, and (4) de-alloying of bimetallic alloys. However, a complete understanding of the ORR kinetics on Pt, the best single element catalyst, and of its low efficiency, is yet to be achieved. These problems, compounded with the high Pt content in current cathode catalysts, and with their gradual loss of performance under operating conditions, still hamper commercialization of fuel cells. In order to minimize the amount of noble metal electrocatalysts and maximize their utilization, while achieving high catalytic activity, numerous synthetic approaches have been attempted. The electrocatalysts were prepared using vacuum deposition methods, wet chemistry methods, or electrodeposition techniques. Electrodeposition in particular has several attractive features with respect to the application in catalyst synthesis such as simplicity of operation and ease of control of the deposition conditions. In this article we describe the application of metal electrodeposition in the synthesis of a new type of electrocatalysts comprising a Pt monolayer (Pt{sub ML}) on metal or alloy nanoparticles. The concept of Pt{sub ML} electrocatalysts offers a possible solution to the impasse caused by a slow ORR kinetics and the consequent large Pt content of conventional electrocatalysts. A Pt{sub ML} shell on a nanoparticle substrate core ensures that every Pt atom is available for catalytic activity; in other words, a Pt{sub ML} achieves the ultimate reduction in Pt loading and complete Pt utilization. Also, through geometric and electronic interaction with the substrate a Pt{sub ML} can change its electronic properties and be more active and durable than pure-Pt electrocatalysts.

30 DIRECT ENERGY CONVERSION↗
DOE OSTI2012

Simulating Cellulose Structure, Properties, Thermodynamics, Synthesis, and Deconstruction with Atomistic and Coarse-Grain Models

Cellulose is still a mysterious polymer in many ways: structure of microfibrils, thermodynamics of synthesis and degradation, and interactions with other plant cell wall components. Our aim is to uncover the details and mechanisms of cellulose digestion and synthesis. We report the details of the structure of cellulose 1-beta under several temperature conditions and report here the results of these studies and connections to experimental measurements and the measurement in-silico the free energy of decrystallization of several morphologies of cellulose. In spatially large modeling, we show the most recent work of mapping atomistic and coarse-grain models into tomographic images of cellulose and extreme coarse-grain modeling of interactions of large cellulase complexes with microfibrils. We discuss the difficulties of modeling cellulose and suggest future work both experimental and theoretical to increase our understanding of cellulose and our ability to use it as a raw material for fuels and materials.

36 MATERIALS SCIENCE↗
DOE OSTI2012

Flow-Solution-Liquid-Solid Growth of Semiconductor Nanowires: A Novel Approach for Controlled Synthesis

Semiconductor nanowires (SC-NWs) have potential applications in diverse technologies from nanoelectronics and photonics to energy harvesting and storage due to their quantum-confined opto-electronic properties coupled with their highly anisotropic shape. Here, we explore new approaches to an important solution-based growth method known as solution-liquid-solid (SLS) growth. In SLS, molecular precursors are reacted in the presence of low-melting metal nanoparticles that serve as molten fluxes to catalyze the growth of the SC-NWs. The mechanism of growth is assumed to be similar to that of vapor-liquid-solid (VLS) growth, with the clear distinctions of being conducted in solution in the presence of coordinating ligands and at relatively lower temperatures (<300 C). The resultant SC-NWs are soluble in common organic solvents and solution processable, offering advantages such as simplified processing, scale-up, ultra-small diameters for quantum-confinement effects, and flexible choice of materials from group III-V to groups II-VI, IV-VI, as well as truly ternary I-III-VI semiconductors as we recently demonstrates. Despite these advantages of SLS growth, VLS offers several clear opportunities not allowed by conventional SLS. Namely, VLS allows sequential addition of precursors for facile synthesis of complex axial heterostructures. In addition, growth proceeds relatively slowly compared to SLS, allowing clear assessments of growth kinetics. In order to retain the materials and processing flexibility afforded by SLS, but add the elements of controlled growth afforded by VLS, we transformed SLS into a flow based method by adapting it to synthesis in a microfluidic system. By this new method - so-called 'flow-SLS' (FSLS) - we have now demonstrated unprecedented fabrication of multi-segmented SC-NWs, e.g., 8-segmented CdSe/ZnSe defined by either compositionally abrupt or alloyed interfaces as a function of growth conditions. In addition, we have studied growth rates as a function of catalyst size/SC-NW diameter and shown for the first time that SLS is governed by Gibbs-Thomson effects. Lastly, from an applications standpoint, we report growth of SC-NWs from a range of substrates, including ITO-coated glass for fabrication of hybrid photovoltaic devices, comparing these to their quasi zero-dimensional quantum-dot counterparts.

36 MATERIALS SCIENCE↗
DOE OSTI2011

Synthesis of mesoporous zeolite single crystals with cheap porogens

Mesoporous zeolite (silicalite-1, ZSM-5, TS-1) single crystals have been successfully synthesized by adding soluble starch or sodium carboxymethyl cellulose (CMC) to a conventional zeolite synthesis system. The obtained samples were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), transmission electron microscopy (TEM), nitrogen sorption analysis, {sup 27}Al magic angle spinning nuclear magnetic resonance ({sup 27}Al MAS NMR), temperature-programmed desorption of ammonia (NH{sub 3}-TPD) and ultraviolet-visible spectroscopy (UV-vis). The SEM images clearly show that all zeolite crystals possess the similar morphology with particle size of about 300 nm, the TEM images reveal that irregular intracrystal pores are randomly distributed in the whole crystal. {sup 27}Al MAS NMR spectra indicate that nearly all of the Al atoms are in tetrahedral co-ordination in ZSM-5, UV-vis spectra confirm that nearly all of titanium atoms are incorporated into the framework of TS-1. The catalytic activity of meso-ZSM-5 in acetalization of cyclohexanone and meso-TS-1 in hydroxylation of phenol was also studied. The synthesis method reported in this paper is cost-effective and environmental friendly, can be easily expended to prepare other hierarchical structured zeolites. - Graphical abstract: Mesoporous zeolite single crystals were synthesized by using cheap porogens as template. Highlights: > Mesoporous zeolite (silicalite-1, ZSM-5, TS-1) single crystals were synthesized. > Soluble starch or sodium carboxymethyl cellulose (CMC) was used as porogens. > The mesoporous zeolites had connected mesopores although closed pores existed. > Higher catalytic activities were obtained.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2012

Large-scale controllable synthesis of dumbbell-like BiVO{sub 4} photocatalysts with enhanced visible-light photocatalytic activity

The controllable synthesis of novel dumbbell-like BiVO{sub 4} hierarchical nanostructures has been successfully obtained via a simple hydrothermal route. The as-synthesized products were studied by X-ray powder diffraction, scanning electron microscopy, transmission electron microscopy and UV-vis absorption spectroscopy. The results showed that the nucleation and growth of the nanodumbbells were governed by an oriented aggregation growth mechanism. It is noteworthy that the concentration of poly(vinyl pyrrolidone) and the volume ratio of H{sub 2}O to CH{sub 3}COOH were crucial to the growth of the final nanoarchitectures. Control experiments were also carried out to investigate the factors which impact on the morphology of the products. Furthermore, the as-prepared BiVO{sub 4} hierarchical nanostructures demonstrated the superior visible-light-driven photocatalytic efficiency, which is helpful for the separation and recycle considering their promising applications in harmful pollutants disposal. - Graphical Abstract: The controllable synthesis of novel dumbbell-like BiVO{sub 4} hierarchical nanostructures has been successfully obtained via a simple hydrothermal route; the as-prepared BiVO{sub 4} hierarchical nanostructures demonstrated the superior visible-light-driven photocatalytic efficiency. Highlights: Black-Right-Pointing-Pointer Dumbbell-like BiVO{sub 4} structures were synthesized and characterized for the first time. Black-Right-Pointing-Pointer The volume ratios of H{sub 2}O to CH{sub 3}COOH were crucial to the final morphologies. Black-Right-Pointing-Pointer Their photocatalytic activity was up to 90% under visible-light irradiation. Black-Right-Pointing-Pointer Dumbbell-like BiVO{sub 4} structures may utilize the pollutant disposal.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗