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At least 1,585 records · Page 88
All sourcesNASA NTRSDOE OSTI
DOE OSTI2012

A Facile Synthesis of MPd (M=Co, Cu) Nanoparticles and Their Catalysis for Formic Acid Oxidation

Monodisperse CoPd nanoparticles (NPs) were synthesized and studied for catalytic formic acid (HCOOH) oxidation (FAO). The NPs were prepared by coreduction of Co(acac)2 (acac = acetylacetonate) and PdBr2 at 260 C in oleylamine and trioctylphosphine, and their sizes (5-12 nm) and compositions (Co10Pd90 to Co60Pd40) were controlled by heating ramp rate, metal salt concentration, or metal molar ratios. The 8 nm CoPd NPs were activated for HCOOH oxidation by a simple ethanol wash. In 0.1 M HClO4 and 2 M HCOOH solution, their catalytic activities followed the trend of Co50Pd50 > Co60Pd40 > Co10Pd90 > Pd. The Co50Pd50 NPs had an oxidation peak at 0.4 V with a peak current density of 774 A/gPd. As a comparison, commercial Pd catalysts showed an oxidation peak at 0.75 V with peak current density of only 254 A/gPd. The synthesis procedure could also be extended to prepare CuPd NPs when Co(acac)2 was replaced by Cu(ac)2 (ac = acetate) in an otherwise identical condition. The CuPd NPs were less active catalysts than CoPd or even Pd for FAO in HClO4 solution. The synthesis provides a general approach to Pd-based bimetallic NPs and will enable further investigation of Pd-based alloy NPs for electro-oxidation and other catalytic reactions.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2015

Solution Phase Synthesis of Indium Gallium Phosphide Alloy Nanowires

The tunable physical and electronic structure of III–V semiconductor alloys renders them uniquely useful for a variety of applications, including biological imaging, transistors, and solar energy conversion. However, their fabrication typically requires complex gas phase instrumentation or growth from high-temperature melts, which consequently limits their prospects for widespread implementation. Furthermore, the need for lattice matched growth substrates in many cases confines the composition of the materials to a narrow range that can be epitaxially grown. In this work, we present a solution phase synthesis for indium gallium phosphide (In x Ga 1–x P) alloy nanowires, whose indium/gallium ratio, and consequently, physical and electronic structure, can be tuned across the entire x = 0 to x = 1 composition range. We demonstrate the evolution of structural and optical properties of the nanowires, notably the direct to indirect band gap transition, as the composition is varied from InP to GaP. Our scalable, low-temperature synthesis affords compositional, structural, and electronic tunability and can provide a route for realization of broader In x Ga 1–x P applications.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Ion correlations explain kinetic selectivity in diffusion-limited solid-state synthesis reactions

Establishing viable solid-state synthesis pathways for novel inorganic materials remains a major challenge in materials science. Previous pathway design methods using pairwise reaction approaches have navigated the thermodynamic landscape with first-principles data but lack kinetic information, limiting their effectiveness. This gap leads to suboptimal precursor selection and predictions, especially for reactions forming competing phases with similar formation energies, where ion diffusion is a critical influence. Here we demonstrate an inorganic synthesis framework by incorporating machine learning-derived transport properties through ‘liquid-like’ product layers into a thermodynamic cellular reaction model. In the Ba–Ti–O system, known for its competitive polymorphism, we obtain accurate predictions of phase formation with varying BaO:TiO2 ratios as a function of time and temperature. We find that diffusion–thermodynamics interplay governs phase compositions, with cross-ion transport coefficients critical for predicting diffusion-limited selectivity. This work bridges length scales and timescales by integrating solid-state reaction kinetics with first-principles thermodynamics and spatial reactivity.

Atomistic models↗
DOE OSTI2012

External field-assisted solution synthesis and selectively catalytic properties of amorphous iron nanoplatelets

This work describes an easy and flexible approach for the synthesis of 2D nanostructures by external composite field-induced self-assembly. Amorphous iron nanoplatelets with a large aspect ratio were prepared by reducing a concentrated FeSO4 solution with NaBH4 without any templates or surfactants under a magnetic field and a shear field, and characterized by field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), selected area electron diffraction (SAED), energy dispersive X-ray spectroscopy (EDX) and X-ray diffraction (XRD). Based on the morphological dependence of the resultant iron nanostructures on the kinetic parameters such as reactant concentration, reaction temperature, external fields as well as reaction time, etc., a novel conceivable formation mechanism of the iron nanoplatelets was substantiated to be a self-assembly of concentrated iron nuclei induced by the synergistic effect of both a magnetic field and a shear field. Due to the amorphous nature and shape anisotropy, the as-synthesized iron nanoplatelets exhibit quite different magnetic properties with an enhanced coercivity of >220 Oe from isotropic iron nanoparticles. In the oxidation of cyclohexane with hydrogen peroxide as a 'green' oxidant, the as-obtained amorphous iron nanoplatelets show a conversion more than 84% and a complete selectivity for cyclohexanol and cyclohexanone due to the unique structure. Moreover, their catalytic performances are strongly influenced by their morphology, and the iron atoms located on the faces tend to catalyze the formation of cyclohexanol while those on the sides tend to catalyze the formation of cyclohexanone. The external composite field-induced solution synthesis reported here can be readily explored for fabricating other 2D magnetic nanoplatelets, and the resulting iron nanoplatelets are promising for a number of applications such as high efficient selective catalysis, energy, environment fields and so forth.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2019

Low-temperature synthesis of all-inorganic perovskite nanocrystals for UV-photodetectors

Controllable synthesis of tin-doped all-inorganic perovskite (e.g. CsPb 1-X Sn X Br 3 ) nanocrystals while maintaining tin at the divalent state is of great importance for tuning their optoelectronic properties by changing the chemical composition and geometrical size; however, this remains a non-negligible challenge. In contrast to the conventional high-temperature (>150 °C) synthesis reaction that would more likely facilitate oxidation of divalent Sn 2+ to quadrivalent Sn 4+ , this work demonstrates a facile low-temperature (105–150 °C) hot-injection method to synthesize quantum-confined Sn 2+ -doped CsPb 1-X Sn X Br 3 nanocrystals with sizes ranging from ~6.2 nm to ~8.3 nm depending on the reaction temperature. The optimized reaction temperature of 135 °C led to a Sn 2+ -doping ratio of 3.4% in CsPb 1-X Sn X Br 3 nanocrystals which exhibited uniform nanoplatelets with an average lateral size of ~7.4 nm. Furthermore, for the first time, we show that the perovskite nanocrystals are promising for the development of low-cost and trap-assisted photomultiplication UV-photodetectors, and the photodetectors based on CsPb 0.966 Sn 0.034 Br 3 nanocrystals exhibited wavelength-dependent detectivities in the magnitude of 1011 Jones for UV light extending from 310 nm to 400 nm at a reverse bias of -7 V. Finally, the high EQE of ~1940% at around 340 nm indicates that the devices had a gain at the large reverse bias condition, which is attributed to the formation of interfacial traps by CsPb 0.966 Sn 0.034 Br 3 nanocrystals that can make the electron injection barrier thin enough to allow electron tunneling in the photodetectors for photomultiplication.

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

Selective sequential infiltration synthesis of ZnO in the liquid crystalline phase of silicon-containing rod-coil block copolymers

The combination of block copolymer (BCP) thin film self-assembly and selective infiltration synthesis of inorganic materials into one BCP block provides access to various organic–inorganic hybrids. Here, we apply sequential infiltration synthesis, a vapor-phase hybridization technique, to selectively introduce ZnO into the organic microdomains of silicon-containing rod-coil diblock copolymers and a triblock terpolymer, polydimethylsiloxane (PDMS)-b-poly{2,5-bis[(4-methoxyphenyl)-oxycarbonyl]styrene} (PDMS-b-PMPCS) and PDMS-b-polystyrene-b-PMPCS (PDMS-b-PS-b-PMPCS), in which the PMPCS rod block is a liquid crystalline polymer. The in-plane cylindrical PDMS-b-PMPCS and core–shell cylindrical and hexagonally perforated lamellar PDMS-b-PS-b-PMPCS films were infiltrated with ZnO with high selectivity to the PMPCS. The etching contrast between PDMS, PS and the ZnO-infused PMPCS enables the fabrication of ZnO/SiO x binary composites by plasma etching and reveals the core–shell morphology of the triblock terpolymer.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Techno-economic and life cycle analyses of the synthesis of a platinum–strontium titanate catalyst

The heterogeneous platinum/strontium titanate (Pt/SrTiO 3 or Pt/STO) catalyst has garnered significant attention as a promising candidate for the hydrogenolysis of polyolefins to hydrocarbon oils. This study evaluates the cost and environmental impacts of a newly developed scalable Pt/STO catalyst production, which includes the synthesis of the STO support and the deposition of Pt onto the support. This two-step synthesis plays a significant role in assessing the commercial feasibility of the catalyst, while energy consumption during the process plays an important role in its environmental impacts. The CatCost and the Research and Development Greenhouse Gases, Regulated Emissions, and Energy use in Technologies (R&D GREET) models were used, respectively, to perform techno-economic analysis (TEA) and life cycle analysis (LCA) of the newly developed catalyst. The TEA showed that the raw materials, accounting for approximately 76% of the total operation cost, has a profound effect on the estimated catalyst cost, mainly due to the platinum precursor. The LCA findings indicated that the catalyst production generates greenhouse gas (GHG) emissions of 66 kg CO 2 e per kg, primarily due to the use of solvents and electricity in the process. The sensitivity analysis indicated that the total operating costs (OpEX), platinum precursor cost, and spent catalyst value (SCV) significantly impact the cost of the synthesized catalyst. Additionally, adopting solvent recovery strategies and using renewable electricity can reduce the GHG emissions of catalyst production to 29 kg CO 2 e per kg.

Heterogeneous Platinum/strontium titanate Catalyst↗
DOE OSTI2011

Direct Synthesis of Fe-Pt Nanoparticles in Ordered Face Centered (fct)LI{sub o} Phase by Microwave Assisted Route

In the present work, microwave-assisted chemical reduction route has been explored for the direct synthesis of fct LIo-phase of Fe-Pt nanoparticles. Effects of microwave power and irradiation time on the growth process were investigated. Using this facile and high yield technique we could tune particle size from 7 to 17 nm. The as-prepared FePt were found to be sensitive to the microwave irradiation power, while influence of exposure time was insignificant. The hysteresis measurements were performed at room temperature (300 K) to study magnetic properties of as-synthesized Fe-Pt as a function of crystallize size. The coercivity and saturation magnetization was observed to be decrease with diminishing for direct synthesis of metal alloys.

36 MATERIALS SCIENCE↗
DOE OSTI2012

Nonlinear damage effect in graphene synthesis by C-cluster ion implantation

We present few-layer graphene synthesis by negative carbon cluster ion implantation with C{sub 1}, C{sub 2}, and C{sub 4} at energies below 20 keV. The small C-clusters were produced by a source of negative ion by cesium sputtering with medium beam current. We show that the nonlinear effect in cluster-induced damage is favorable for graphene precipitation compared with monomer carbon ions. The nonlinear damage effect in cluster ion implantation shows positive impact on disorder reduction, film uniformity, and the surface smoothness in graphene synthesis.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2013

Controlled synthesis of buried delta-layers of Ag nanocrystals for near-field plasmonic effects on free surfaces

We report on the shallow synthesis by low energy ion implantation of delta-layers of Ag nanocrystals in SiO{sub 2} at few nanometers under its free surface. Transmission electron microscopy observations, ballistic simulations, and reflectance measurements are coupled to define the conditions for which the synthesis is fully controlled and when, on the contrary, this control is lost. We show that low dose implantation leads to the formation of a well-defined single plane of nanocrystals, while for larger doses, sputtering and diffusion effects limit the control of the size, position, and volume amount of these nanocrystals. This paper provides the experimental evidence of the incorporated dose saturation predicted in the literature when implanting metal ions at high doses in glass matrices. Its consequences on the particle population and the plasmonic optical response of the composite layers are carefully analyzed. We show here that this saturation phenomenon is underestimated in standard simulation predictions due to diffusion of metal atoms towards the surface and nanocrystal nucleation during the implantation process.

36 MATERIALS SCIENCE↗
DOE OSTI2013

Controlled synthesis of nickel ferrite nanocrystals with tunable properties using a novel induction thermal plasma method

Nickel ferrite spinel nanopowders were synthesised using a solution spray radio-frequency inductively coupled plasma reactor over a wide range of compositions (Ni{sub x}Fe{sub 3-x}O{sub 4}, x ≤ 1), with metastable powders produced for x = 0, 0.25, and 0.5. X-ray fluorescence and X-ray diffraction coupled to Rietveld refinement show that this synthesis technique offers an excellent level of control over both the chemical and crystallographic composition of the nanopowder through the control of the input Fe/Ni ratio. The technique produces highly crystalline nanopowders without the need for post-synthesis annealing. A bulk Fe/Ni ratio ≥2 yields a pure spinel Ni{sub x}Fe{sub 3-x}O{sub 4} phase, whereas Fe/Ni ratio <2 results in the excess Ni partitioning to a secondary bunsenite (Ni{sub x},Fe{sub 1-x})O phase. Morphological analysis using transmission electron microscopy shows that two types of particles are produced in different parts of the reactor: a highly faceted powder with the truncated octahedron morphology and a smaller-sized random agglomerate. The faceted particles have a log-normal particle size distribution, with an average size of about 30 nm while the agglomerates have a characteristic length of ∼3–5 nm.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Silver nanoplates with ground or metastable structures obtained from template-free two-phase aqueous/organic synthesis

Silver has unique electrical, catalytic, and plasmonic characteristics and has been widely sought for fabrication of nanostructures. The properties of silver nanostructures are intimately coupled to the structure of silver crystals. Two crystal structures are known for silver: the stable (ground) state cubic face centered 3C-Ag structure and the metastable hexagonal 4H-Ag structure. Recently, Chackraborty et al. [J. Phys.: Condens. Matter 23, 325401 (2011)] discovered a low density, highly reactive metastable hexagonal 2H-Ag structure accessible during electrodeposition of silver nanowires in porous anodic alumina templates. This 2H-Ag structure has enhanced electrical and catalytic characteristics. In the present work we report template-free synthesis of silver nanoplates with the metastable 2H-Ag crystal structure, which appears together with the ground 3C-Ag and the metastable 4H-Ag structures in a two-phase solution synthesis with citric acid as the capping agent. The capacity of citric acid to stabilize both the stable and the metastable structures is explained by its preferential binding to the close packed facets of Ag crystals, which are the (111) planes for 3C-Ag and the (0001) planes for 4H-Ag and 2H-Ag. Nanoplate morphology and structure are characterized using scanning electron microscopy, X-ray diffraction, and transmission electron microscopy. The synthesized nanoplates have thickness from 15 to 17 nm and edge length from 1 to 10 μm. Transmission electron microscopy selected area electron diffraction is used to uniquely identify and distinguish between nanoplates with 2H-Ag or 4H-Ag or 3C-Ag structures.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2014

Synthesis and magnetic properties of single phase titanomagnetites

The focus of this paper is the study of cation distributions and resulting magnetizations in titanomagnetites (TMs), (1−x)Fe{sub 3}O{sub 4−x}Fe{sub 2}TiO{sub 4} solid solutions. TM remnant states are hypothesized to contribute to planetary magnetic field anomalies. This work correlates experimental data with proposed models for the TM pseudobinary. Improved synthesis procedures are reported for single phase Ulvöspinel (Fe{sub 2}TiO{sub 4}), and TM solid solutions were made using solid state synthesis techniques. X-ray diffraction and scanning electron microscopy show samples to be single phase solid solutions. M-H curves of TM75, 80, 85, 90, and 95 (TMX where X = at. % of ulvöspinel) were measured using a Physical Property Measurement System at 10 K, in fields of 0 to 8 T. The saturation magnetization was found to be close to that predicted by the Neel model for cation distribution in TMs. M-T curves of the remnant magnetization were measured from 10 K to 350 K. The remnant magnetization was acquired at 10 K by applying an 8 T field and then releasing the field. Experimental Neel temperatures are reported for samples in the Neel model ground state.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2014

Electrochemical synthesis of nanosized hydroxyapatite by pulsed direct current method

Synthesis of nanosized of hydroxyapatite (HA) by electrochemical pulsed direct current (PDC) method has been studied. The aim of this work is to study the influence of various PDC parameters (pH initial, electrode distance, duty cycle, frequency, and amplitude) on particle surface area of HA powders. The electrochemical synthesis was prepared in solution Ca{sup 2+}/EDTA{sup 4−}/PO{sub 4}{sup 3+} at concentration 0.25/0.25/0.15 M for 24 h. The electrochemical cell was consisted of two carbon rectangular electrodes connected to a function generator to produce PDC. There were two treatments for particles after electrosynthesized, namely without aging and aged for 2 days at 40 °C. For both cases, the particles were filtered and washed by demineralized water to eliminate the impurities and unreacted reactants. Then, the particles were dried at 100 °C for 2 days. The dried particles were characterized by X-ray diffraction, surface area analyzer, scanning electron microscopy (SEM), Fourier transform infrared spectra and thermogravimetric and differential thermal analysis. HA particles can be produced when the initial pH > 6. The aging process has significant effect on the produced HA particles. SEM images of HA particles showed that the powders consisted of agglomerates composed of fine crystallites and have morphology plate-like and sphere. The surface area of HA particles is in the range of 25 – 91 m{sup 2}/g. The largest particle surface area of HA was produced at 4 cm electrode distance, 80% cycle duty, frequency 0.1 Hz, amplitude 9 V and with aging process.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2014

Large-scale synthesis of Ba{sub x}Sr{sub 1−x}TiO{sub 3} nanowires with controlled stoichiometry

This study demonstrates a highly efficient method for large-scale synthesis BaTiO{sub 3} nanowires (NWs) using a two-step hydrothermal reaction. This synthesis process provides a facile approach to the growth of BaTiO{sub 3} NWs with high yield and control over the stoichiometry of the Ba{sub x}Sr{sub 1−x}TiO{sub 3} solid solution. The ferroelectricity of the BaTiO{sub 3} NWs is directly characterized using atomic force microscopy with the piezoelectric strain coupling coefficient (d{sub 33}) reaching 31.1 pm/V. This work provide an avenue for high volume manufacturing of ferroelectric NWs, allowing both fundamental investigation of nanoscale ferroelectricity as well as their future application in the electrical devices.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Thermal plasma synthesis of Fe{sub 1−x}Ni{sub x} alloy nanoparticles

Fe-Ni alloy nanoparticles are of great interest because of diverse practical applications in the fields such as magnetic fluids, high density recording media, catalysis and medicine. We report the synthesis of Fe-Ni nanoparticles via thermal plasma route. Thermal plasma assisted synthesis is a high temperature process and gives high yields of production. Here, we have used direct arc thermal plasma plume of 6kw as a source of energy at operating pressure 500 Torr. The mixture of Fe-Ni powder in required proportion (Fe{sub 1−x}Ni{sub x}; x=0.30, 0.32, 0.34, 0.36, 0.38 and 0.40) was made to evaporate simultaneously from the graphite anode in thermal plasma reactor to form Fe-Ni bimetallic nanoparticles. The as synthesized particles were characterized by X-Ray Diffraction (XRD), Thermo-Gravimetric Analysis/Differential Scanning Calorimtry (TGA/DSC)

36 MATERIALS SCIENCE↗
DOE OSTI2014

Synthesis and characterization of 10 nm thick piezoelectric AlN films with high c-axis orientation for miniaturized nanoelectromechanical devices

The scaling of piezoelectric nanoelectromechanical systems (NEMS) is challenged by the synthesis of ultrathin and high quality piezoelectric films on very thin electrodes. We report the synthesis and characterization of the thinnest piezoelectric aluminum nitride (AlN) films (10 nm) ever deposited on ultrathin platinum layers (2–5 nm) using reactive sputtering. X-ray diffraction, high-resolution transmission electron microscopy, and fast Fourier transform analyses confirmed the proper crystal orientation, fine columnar texture, and the continuous lattice structure within individual grains in the deposited AlN nanometer thick films. The average extracted d{sub 31} piezoelectric coefficient for the synthesized films is −1.73 pC/N, which is comparable to the reported values for micron thick and highly c-axis oriented AlN films. The 10 nm AlN films were employed to demonstrate two different types of optimized piezoelectric nanoactuators. The unimorph actuators exhibit vertical displacements as large as 1.1 μm at 0.7 V for 25 μm long and 30 nm thick beams. These results have a great potential to realize miniaturized NEMS relays with extremely low voltage, high frequency resonators, and ultrasensitive sensors.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2014

Synthesis and properties of ferromagnetic nanostructures embedded within a high-quality crystalline silicon matrix via ion implantation and nanocavity assisted gettering processes

Integrating magnetic functionalities with silicon holds the promise of developing, in the most dominant semiconductor, a paradigm-shift information technology based on the manipulation and control of electron spin and charge. Here, we demonstrate an ion implantation approach enabling the synthesis of a ferromagnetic layer within a defect free Si environment by exploiting an additional implant of hydrogen in a region deep below the metal implanted layer. Upon post-implantation annealing, nanocavities created within the H-implanted region act as trapping sites for gettering the implanted metal species, resulting in the formation of metal nanoparticles in a Si region of excellent crystal quality. This is exemplified by the synthesis of magnetic nickel nanoparticles in Si implanted with H{sup +} (range: ∼850 nm; dose: 1.5 × 10{sup 16 }cm{sup −2}) and Ni{sup +} (range: ∼60 nm; dose: 2 × 10{sup 15 }cm{sup −2}). Following annealing, the H implanted regions populated with Ni nanoparticles of size (∼10–25 nm) and density (∼10{sup 11}/cm{sup 2}) typical of those achievable via conventional thin film deposition and growth techniques. In particular, a maximum amount of gettered Ni atoms occurs after annealing at 900 °C, yielding strong ferromagnetism persisting even at room temperature, as well as fully recovered crystalline Si environments adjacent to these Ni nanoparticles. Furthermore, Ni nanoparticles capsulated within a high-quality crystalline Si layer exhibit a very high magnetic switching energy barrier of ∼0.86 eV, an increase by about one order of magnitude as compared to their counterparts on a Si surface or in a highly defective Si environment.

36 MATERIALS SCIENCE↗