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A robust electrodeposition method consisting of the rotating disk slurry electrode (RoDSE) technique to obtain Au nanoparticles highly dispersed on a conductive carbonaceous support, i.e., Vulcan XC-72R, for ethanol electrooxidation reaction in alkaline media was developed. Ceria was used as a cocatalyst using a Ce(III)-EDTA impregnation method in order to enhance the catalytic activity and improve the catalyst’s overall stability. The RoDSE method used to obtain highly dispersed Au nanoparticles does not require the use of a reducing agent or stabilizing agent, and the noble-metal loading was controlled by the addition and tuning of the metal precursor concentration. Inductively coupled plasma and thermogravimetric analysis indicated that the Au loading in the catalyst was 9 %. Particle size and characteristic Au fcc crystal facets were determined by X-ray diffraction. The morphology of the catalyst was also investigated using electron microscopy techniques. In addition, X-ray absorption spectroscopy was used to corroborate the presence and identify the oxidation state of Ce in the system and to observe if there are any electronic interactions within the 8 % Au/CeOx/C system. Cyclic voltammetry of electrodeposited 9 % Au/C and Ce-promoted 8 % Au/C showed a higher catalytic current density for ethanol oxidation when compared with commercially available catalysts (20 % Au/C) of a higher precious metal loading. In addition, we report a higher stability toward the ethanol electrooxidation process, which was corroborated by 1 mV/s linear sweep voltammetry and chronoamperometric studies.

Aggregation of magnetic nanoparticles in polymer melts was assessed using dynamic magnetic susceptibility measurements. Magnetic nanocomposites consisting of polybutadiene/CoFe2O4 and polystyrene/CoFe2O4 mixtures were prepared using different techniques and characterized using dynamic magnetic susceptibility measurements. The presence of nanoparticle aggregates determined using magnetic measurements was confirmed with transmission electron microscopy examinations. The results were in good agreement with predictions from the Flory–Huggins interaction parameters.

The synthesis of a polyaniline–clay nanocomposite (PAniC NC) was achieved using the in situ polymerization of aniline in a Cloisite® 30B nanoclay suspension in a supercritical CO2 (Sc-CO2) medium. The interfacial co-polymerization of aniline (ANI) and m-aminobenzenesulfonic acid (SAN) in the presence of Cloisite® 30B was performed in Sc-CO2/water to produce the SPANI-clay NC. The NC was then mixed with a water-based hardener. This water-based composite is developed with the goal of reducing environmental and health risks. The use of this Sc-CO2 technique produced a composite material that resulted in the enhanced protection of carbon steel against corrosion when compared to a similar composite synthesized under atmospheric conditions. The materials obtained were characterized using UV/visible spectroscopy, X-ray powder diffraction and scanning and transmission electron microscopy. The anti-corrosion performance and the adhesion properties of these coatings were evaluated using standardized tests. Electrochemical impedance spectroscopy was also used to determine the electrochemical properties of these anti-corrosion coatings. Better exfoliation and dispersion of the clay was achieved using the Sc-CO2 medium resulting in superior performances in corrosion and electrochemical tests because of the higher level of intercalation.

Platinum was electrodeposited onto Y-zeolite and Y-zeolite (Y)/Vulcan XC-72R (V) to produce Pt/Y/V and Pt/Y catalysts using a rotating disk slurry electrode technique. The activities of the two catalysts were measured towards methanol electro-oxidation in alkaline media by cyclic voltammetry and chronoamperometry. The materials were examined using electron microscopy. The results were compared to those obtained on commercial catalysts. Pt/Y/V (with 14 wt% Pt) catalyst was the most active, even more so than a commercial Pt/V catalyst with 20 wt% Pt. The Pt/Y/V catalysts contained Pt nanoparticles and tetrahedra, likely a consequence of the nucleation and growth within the zeolite framework.

In this study we probe the electrocatalytic activity of Pt nanoparticles supported on ceria nanoparticles (NPs) and nanorods (NRs) in the ethanol oxidation reaction (EOR) in alkaline media. The goal of this study was to relate morphology, support structure and composition to the EOR catalytic activity by using in situ X-ray absorption fine structure (XAFS) studies. Cyclic voltammetry experiments showed that both ceria supported catalysts (NP vs. NR) had similar peak current densities at fast scan rates, however at slow scan rates, the ceria NR catalyst showed superior catalytic activity. In situ XAFS studies in KOH showed that both ceria supported catalysts had more electron density in their d-band (with the ceria NR having more electron density overall) than ceria - free Pt/Vulcan standard. However, in an ethanol solution the ceria NR catalyst had the least electron density. We propose that this change is due to the increased charge transfer efficiency between the ceria nanorod support and platinum. In the KOH solution, the increased electron density makes the platinum less electrophilic and hinders Pt-OH bond formation. In the EtOH solution, platinum's increased nucleophilicity facilitates the bond formation between Pt and the electron deficient carbon in ethanol which in turn withdraws the electron density from platinum and increases the white line intensity as observed in the XAS measurements.

We demonstrate that layered carbon black nanoparticles can be oxidatively peeled via the reaction with potassium permanganate in sulfuric acid. As a result of this reaction, outer layers of carbon nanoparticles “peel” off due to high levels of oxidation while the less oxidized inner cores, though they exhibit remarkable solubility in water, remain mostly intact.

Multi-walled carbon nanotubes (MWCNTs) dispersed onto a silicon substrate have been coated with diamond nanocrystals (DNC) and silicon carbide (SiC) from solid carbon and silicon sources exposed to H2 activated by hot filament chemical vapor deposition (HFCVD) at around 190 °C substrate temperature. MWCNT coating by DNC initiates during filament carburization process at 80 °C substrate temperature under conventional HFCVD conditions. The hybrid nanocarbon material was analyzed by scanning electron microscopy, transmission electron microscopy, energy dispersive X-ray spectroscopy, electron energy loss spectroscopy, selected area electron diffraction, X-ray diffraction and Raman spectroscopy. The structure of the MWCNTs is preserved during coating and the smooth DNC/SiC coating is highly conformal. The average grain size is below 10 nm. The growth mechanism of DNC and SiC onto MWCNT surface is discussed.

Precipitates (ppts) in new generation aluminum-lithium alloys (AA2099 and AA2199) were characterised using scanning and transmission electron microscopy and atom probe tomography. Results obtained on the following ppts are reported: Guinier-Preston zones, T1 (Al2 CuLi), β' (Al3 Zr) and δ' (Al3 Li). The focus was placed on their composition and the presence of minor elements. X-ray energy-dispersive spectrometry in the electron microscopes and mass spectrometry in the atom probe microscope showed that T1 ppts were enriched in zinc (Zn) and magnesium up to about 1.9 and 3.5 at.%, respectively. A concentration of 2.5 at.% Zn in the δ' ppts was also measured. Unlike Li and copper, Zn in the T1 ppts could not be detected using electron energy-loss spectroscopy in the transmission electron microscope because of its too low concentration and the small sizes of these ppts. Indeed, Monte Carlo simulations of EEL spectra for the Zn L2,3 edge showed that the signal-to-noise ratio was not high enough and that the detection limit was at least 2.5 at.%, depending on the probe current. Also, the simulation of X-ray spectra confirmed that the detection limit was exceeded for the Zn Kα X-ray line because the signal-to-noise ratio was high enough in that case, which is in agreement with our observations.

A simple method was used to electrodeposit a metallic coating on vertically aligned carbon nanotube (CNT) arrays, herein referred to as turfs, creating an open cell, core–shell foam. The foam exhibited highly elastic behavior, approaching the amount of elastic recovery in compression of a pure CNT turf. The turfs were pre-treated with an acid bath, and were electroplated at low voltages with nickel and copper. This simple method can be expanded to prepare a large variety of nanostructured foams (e.g., the carbon support can be changed, the metal deposited selected and its thickness controlled) while maintaining their mechanical robustness.

Titanium oxide (TiO2) nanoparticles (NPs) were doped with vanadium using a novel, facile, and inexpensive method. The TiO2 NPs were dispersed in a vanadyl oxalate solution prepared by dissolving vanadium pentoxide (V2O5) in oxalic acid. A short heat treatment at 400 °C applied to the dried mixture resulted in the doping of TiO2 with a net measured decrease of its band gap by about 0.5 eV, making this important semiconductor material usable in the visible light spectrum.

WO3 nano-ribbons: their phase transformation from tungstite (WO3·H2O) to tungsten oxide (WO3)

We report on the magnetothermal repair of a thermoplastic magnetic nanocomposite consisting of iron oxide nanoparticles embedded in poly(methyl methacrylate) (PMMA). The nanoparticles responded to an applied alternating magnetic field by dissipating heat, raising the nanocomposite temperature to above the glass transition temperature and resulting in the repair of the nanocomposite. This was demonstrated by cutting the nanocomposite and subsequently joining two pieces together under the action of an alternating magnetic field. Examination by optical and transmission electron microscopy of the region where the two pieces were joined demonstrated the healing and disappearance of the interface between both pieces down to the nanoscale.

Magnetic polymer colloids (MPCs) consisting of CoFe2O4 nanoparticles (NPs) embedded in a poly(methyl methacrylate) (PMMA) matrix were synthesized by magnetic miniemulsion polymerization. CoFe2O4 NPs were modified with 3-trimethoxysilylpropylmethacrylate and directly emulsified with different concentrations of sodium dodecyl sulfate under ultrasonication for subsequent miniemulsion polymerization. The average diameter of the CoFe2O4/PMMA spheres (about 200 nm) was controlled by varying the amount of surfactant. Thermogravimetric analysis indicated that the magnetic content was in the range of 44 to 73 %. Magnetic properties of the dispersions were investigated by measuring equilibrium magnetization curves and the dynamic magnetic susceptibility as a function of frequency. The MPCs were found to follow the Debye model for the dynamic magnetic susceptibility, with a characteristic time given by the rotational hydrodynamic resistance and thermal energy through the Stokes-Einstein relation. This demonstrates that the MPCs respond to applied magnetic fields by rotating. Due to their uniform size and high magnetic loading, these colloids may be suitable in a variety of applications, including nanoscale mechanical probes and actuators in complex fluids and biological systems.

The catalytic activity of platinum (Pt) nanoparticles (NPs) towards methanol electrooxidation in alkaline media was demonstrated to be dependent on their interactions with their nanostructured ceria support. Ceria nanorods (NRs) with diameters of 5 to 10 nm and lengths of 15 to 50 nm as well as ceria NPs with diameters of 2 to 6 nm were applied as supports for similarly sized Pt NPs with diameters of 2 to 5 nm. Cyclic voltammetry data showed that Pt NPs supported on ceria NPs exhibited a 2-to-5-fold higher catalytic current density versus ceria NRs. X-ray photoelectron spectroscopic data indicated that Pt NPs deposited onto ceria NRs were disproportionally composed of oxidized species (Pt2+, Pt4+ and Pt–O–M) rather than Pt0 while Pt NPs on ceria NPs mainly consisted of Pt0. Stronger metal-support interactions between Pt NPs and ceria NRs are postulated to induce preferential oxidation of Pt NPs and consequently decrease the catalytic sites and overall activity.

We report the optical and vibrational properties of nanocrystalline MoS2 thin films, which are comprised of stripe-like partially edge-terminated vertically aligned (ETVA) nano-size crystals dispersed in ⟨001⟩ oriented regions, grown on large insulating substrates. From high-resolution transmission electron microscopy experiments, the average grain size of ETVA MoS2 layers was found to be ∼5 nm and consist of three to five monolayers. The ETVA and flat nanocrystalline regions were in equivalent proportions in the films. The films were highly transparent (∼80%), but the transmittance decreased as the energy of the incident light approached the band gap. Additionally, weak excitonic peaks were observed in both the absorption and transmission spectra. The room-temperature Raman study showed that the line shape for both E2g1 and A1g modes was significantly broader, and few additional Raman modes were observed in comparison to bulk MoS2. The broadening in the line shape of the A1g mode was analyzed using the p...

We report on the control of cyclotrimerization forming a polycyanurate polymer using magnetic iron oxide nanoparticles in an alternating-current (ac) field as an internal heat source, starting from a commercially available monomer. Magnetic nanoparticles were dispersed in the monomer and catalytic system using sonication, and the mixture was subjected to an alternating magnetic field, causing the magnetic nanoparticles to dissipate the energy of the magnetic field in the form of heat. Internal heating of the particle/monomer/catalyst system was sufficient to start and sustain the polymerization reaction, producing a cyanate ester network with conversion that compared favorably to polymerization through heating in a conventional laboratory oven. The two heating methods gave similar differential scanning calorimetry temperature profiles, conversion rates, and glass transition temperatures when using the same temperature profile. The ability of magnetic nanoparticles in an ac field to drive the curing reaction should allow for other reactions forming high-temperature thermosetting polymers and for innovative ways to process such polymers.

Non-toxic magnetic-luminescent iron oxide Mn2+-doped zinc sulfide (Fe3O4/ZnS:Mn) composite nanoparticles were synthesized through a one-step chemical deposition route using surface-treated Fe3O4 nanoparticles. High resolution electron microscopy and X-ray diffraction analyses showed that the two individual phases co-exist with a high degree of crystalline quality, no parasitic phases were found. The average crystallite size was around 9 nm. At the doping level of 20–25 wt% Mn2+, the luminescence signal of the composite at 598 nm is very intense, comparable to that of ZnS:Mn. This remarkable effect has been evidenced solely for Fe3O4 Cd2+-based composites, which are toxic. Moreover, the superparamagnetic response of Fe3O4 with near-zero coercivity is successfully retained in the composite. This notable bifunctionality of Fe3O4/ZnS:Mn can enable both in vivo and in vitro biomedical applications.

A new approach is presented to introduce the fine structure of core-loss excitations into the electron energy-loss spectra of ionization edges by Monte Carlo simulations based on an optical oscillator model. The optical oscillator strength is refined using the calculated electron energy-loss near-edge structure by density functional theory calculations. This approach can predict the effects of multiple scattering and thickness on the fine structure of ionization edges. In addition, effects of the fitting range for background removal and the integration range under the ionization edge on signal-to-noise ratio are investigated.

Boron nitride nanosheets (BNNSs) have an identical crystal structure and similar lattice parameter to those of graphene sheets. However, growing quality BNNSs consisting of only several atomic layers remains a challenge. Here, we report on the synthesis of BNNSs at a temperature of 350 °C using a CO2 pulsed laser plasma deposition (CO2-PLD) technique by irradiating a pyrolytic hexagonal boron nitride (h-BN) target. The deposition was performed either in vacuum at a pressure of 0.2 Pa, for which we obtained polycrystalline BN, or in hydrogen (H2) atmosphere at a pressure of 26 Pa for which we obtained single-crystal BNNSs. The presence of H2 seems to minimize the side effects of sputtering and the material shows higher purity and better crystallinity. High resolution transmission electron microscopy (HRTEM) showed the sheets to be mostly defect-free and to have the characteristic honeycomb structure of six-membered B3-N3 hexagon. HRTEM, electron diffraction, X-ray diffraction, Raman scattering, and Fourier transform infrared spectroscopy clearly identified h-BN.

Spontaneously detaching self-standing diamond films were successfully fabricated using saturated hydrocarbon polymers as seeding source by hot filament chemical vapor deposition (HFCVD) technique. X-ray diffraction confirmed the crystal structure of diamond. The microcrystalline morphology of the diamond films was analyzed by atomic force microscopy (AFM) and scanning electron microscopy. Raman spectra from the front and back sides of the films show the characteristic diamond band at 1332 cm − 1 and no carbide layer. EELS spectra also show the signature features of diamond. The use of hydrocarbon polymers as seeding source will improve the cost-effectiveness of the fabrication of diamond wafers by simplifying the fabrication process.

A nanofluid is a solid-liquid composite material consisting of a stable suspension of nanometric particles in a conventional refrigerant liquid expected to exhibit enhanced heat transfer properties. Elemental silver (Ag) was selected in this research because of its high electrical and thermal conductivity that are likely to be dependent on the crystal size and shape at the nanoscale. Accordingly, we have synthesized highly monodisperse silver nanowires and nanocrystals by reducing silver nitrate solutions with ethylene glycol in presence of polyvinylpyrrolidone, (PVP). The shape-control in the silver nanostructures was achieved by a proper selection of the type and level of chloride salts, e.g. KCl and CaCl2, and specific PVP/Ag mole ratios in starting solutions. The development of the metal phase was confirmed by X-ray diffractometry. Transmission electron microscopy analyses evidenced the formation of silver nanowires exhibiting a very uniform thickness that could be tuned in the 40-130nm range. UV-vis measurements evidenced the plasmon peak at ∼387nm and clear shoulders at ∼357nm that are indicative of the formation of elongated nanostructures.

We present a scalable, reproducible and economic process for the fabrication of diamond and diamond-graphene hybrid films using paraffin wax as a seeding source for diamond. The films were characterized using Raman spectroscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM), and electron energy loss spectroscopy (EELS). Raman spectra show the characteristic band of diamond at 1332 cm-1 and the D, G, and 2D bands of graphene at 1360, 1582 and 2709 cm-1, respectively. Electron microscopy confirms the microcrystalline nature of the diamond films with crystal size in the range of 0.5 μm to 1.0 μm, and the hybrid film consists of microcrystalline diamond attached to thin, semi-transparent graphene flakes. The graphene-diamond hybrid films exhibit a turn-on field of about 3.6 V/μm with a prolonged current stability of at least 135 h.

The stability and oxygen reduction activity of two carbon-supported catalyst materials are reported. The catalysts, Se/Ru and Se/(Ru-Mo), were prepared by using a chemical reduction method. The catalyst nanoparticles were evenly dispersed onto globular amorphous carbon supports, and their average size was ca. 2.4 nm. Thermal treatment at 500 °C for 2 h in an inert argon atmosphere resulted in coarsening of the nanoparticles, and also in some decrease of their activity. A gradual reduction of activity was also observed for Se/Ru during potential-cycle experiments. However, the incorporation of small amounts of Mo into the Se/Ru catalysts considerably improved the stability of the catalyst against dissolution. The Mo-containing samples showed excellent oxygen reduction activities even after cycling the potential 1000 times between 0.7 and 0.9 V. Furthermore, they showed excellent fuel-cell behavior. The performance of the Se/Ru catalysts is greatly improved by the addition of small amounts of elemental Mo. Possible mechanisms responsible for the improvement of the activity are discussed.

Synchrotron-based X-ray absorption spectroscopy (XAS), including the surface-specific ΔXANES technique, is used to investigate the active reaction site for water activation and the oxygen reduction reaction (ORR) on the novel, mixed-phase chalcogenide electrocatalyst RhxSy/C (De Nora). The specific adsorption of water, OH, and O as a function of overpotential is reported. This study builds on a prior communication based solely on interpreting the XAS spectra of RhxSy with respect to the metallic Rh3S4 phase. Here, a more extensive overview of the electrocatalysis is provided on RhxSy/C, the thermally grown Rh2S3/C and Rh3S4/C preferential phases and a standard 30 wt % Rh/C electrocatalyst, including results obtained by X-ray diffraction (XRD), XAS, high-resolution transmission electron imaging, microanalysis, and electrochemical investigations. Heating of the RhxSy catalysts to prepare the two preferential phases causes Rh segregation and the formation of Rh metal particles, and immersion in TFMSA causes ...

The oxidation of both single crystal and relatively pure polycrystalline silicon carbide, between 973 and 2053 K, resulted in the formation of cristobalite, quartz, or tridymite, which are the stable crystalline polymorphs of silica (SiO2) at ambient pressure. The oxide scales were found to be pure SiO2 with no contamination resulting from the oxidizing environment. The only variable affecting the occurrence of a specific polymorph was the oxidation temperature. Cristobalite was formed at temperatures ≥1673 K, tridymite between 1073 and 1573 K, and quartz formed at 973 K. The polymorphs were determined using electron diffraction in a transmission electron microscope. These results were further confirmed using infrared and Raman spectroscopies. Cristobalite was observed to grow in a spherulitic fashion from amorphous silica. This was not the case for tridymite and quartz, which appeared to grow as oriented crystalline films. The presence of a thin silicon oxycarbide interlayer was detected at the interface between the SiC substrate and the crystalline silica using x-ray photoelectron spectroscopy.

We have shown that the asterism in garnets emanating from Emerald Creek, Latah County, Idaho, is due to the precipitation of acicular crystals in the garnet crystal host. These inclusions have been identified, using electron microscopy, as tetragonal rutile, the stable phase of TiO2. One set of rutile (r) needles was found to have the following crystallographic relationship with its garnet (g) host: \([011]_g /\!/[0\bar 10]_r,(02\bar 2)_g /\!/(100)_r,(\bar 400)_g /\!/(001)_r\). From meticulous examinations of the asteriated garnets and the angular relationships between the rutile inclusions and the garnet matrix it was possible to determine the orientations of the other sets of needles for both four and six rayed star garnets. A six rayed star garnet exhibits needles aligned along the \(\langle 111\rangle\) and \(\langle 011\rangle\) directions of the garnet while a four rayed star garnet exhibits needles aligned along the \(\langle 111\rangle\) directions only. These results are believed to be applicable to asteriated garnets emanating from all sources.

Silicon carbide ceramics have great potential for use in harsh environment applications, however many technical challenges still need to be addressed, including high temperature stability. The oxidation of SiC in air up to temperatures of 2053 K was conducted and resulted in the formation of a thermally grown silica scale that does not prove to be protective for very high temperature applications because of its rapid degradation. Examination of the oxide scale using scanning electron microscopy revealed the presence of striking features formed in a manner analogous to conventional glass blowing techniques. These features occurred for oxidation temperatures of at least 1773 K. The interfacial reaction between SiC and the oxide scale is responsible for the production of gases that must somehow escape. If the viscosity of the silica scale is low enough then it can be deformed freely by this pressure buildup.

Three very different commercial glasses were chosen for their close matched coefficient of thermal expansion with SiC and were tested in view of their application as glass sealants for SiC packages. The occurrence of bubbles at the glass/SiC interface was attributed to the reaction between the SiC substrate and certain oxides present in the glasses forming CO gas. Selection criteria were developed based on thermodynamic calculations in order to determine which glass composition would be stable with SiC. This approach provides valuable information in tailoring suitable glasses for the demanding applications that SiC materials may encounter in packaging for high temperature applications.

Elucidation of the structural transformations in graphene oxide (GO) upon reduction remains an active and important area of research. We report the results of in situ heating experiments, during which electrical, mass spectrometry, X-ray photoelectron spectroscopy (XPS), Raman spectroscopy, and transmission electron microscopy (TEM) measurements were carried out correlatively. The simultaneous electrical and temperature programmed desorption measurements allowed us to correlate the onset of the increase in the electrical conductivity of GO by five orders of magnitude at about 150 °C with the maxima of the rates of desorption of H2O, CO, and CO2. Interestingly, this large conductivity change happens at an intermediate level of the reduction of GO, which likely corresponds to the point when the graphitic domains become large enough to enable percolative electronic transport. We demonstrate that the gas desorption is intimately related to (i) the changes in the chemical structure of GO detected by XPS and Ra...

We report the growth of high indium content InGaN:Yb nanorods grown on c-plane sapphire (0001) substrates using plasma assisted molecular beam epitaxy. The in situ reflection high energy electron diffraction patterns recorded during and after the growth revealed crystalline nature of the nanorods. The nanorods were examined using electron microscopy and atomic force microscopy. The photoluminescence studies of the nanorods showed the visible emissions. The In composition was calculated from x-ray diffraction, x-ray photoelectron spectroscopy, and the photoluminescence spectroscopy. The In-concentration was obtained from photoluminescence using modified Vegard's law and found to be around 37% for InGaN and 38% for Yb (5 ± 1%)-doped InGaN with a bowing parameter b = 1.01 eV. The Yb-doped InGaN showed significant enhancement in photoluminescence properties compared to the undoped InGaN. The Yb-doped InGaN nanorods demonstrated the shifting of the photoluminescence band at room temperature, reducing luminescence amplitude temperature dependent fluctuation, and significant narrowing of excitonic emission band as compared to the undoped InGaN. The magnetic properties measured by superconducting quantum interference devices reveals room temperature ferromagnetism, which can be explained by the double exchange mechanism and magnetostriction.

MoS2 is an important member of the transition metal dichalcogenides that is emerging as a potential 2D atomically thin layered material for low power electronic and optoelectronic applications. However, for MoS2 a critical fundamental question of significant importance is how the surface energy and hence the wettability is altered at the nanoscale in particular, the role of crystallinity and orientation. This work reports on the synthesis of large area MoS2 thin films on insulating substrates (SiO2/Si and Al2O3) with different surface morphology via vapor phase deposition by varying the growth temperatures. The samples were examined using transmission electron microscopy and Raman spectroscopy. From contact angle measurements, it is possible to correlate the wettability with crystallinity at the nanoscale. The specific surface energy for few layers MoS2 is estimated to be about 46.5 mJ/m2. Moreover a layer thickness-dependent wettability study suggests that the lower the thickness is, the higher the contact angle will be. Our results shed light on the MoS2-water interaction that is important for the development of devices based on MoS2 coated surfaces for microfluidic applications. © 2014 American Chemical Society.

Tungstite (WO3.H2O) nanoparticles were synthesized using a simple and inexpensive low temperature and low pressure hydrothermal method by adding hydrochloric acid to diluted sodium tungstate solutions (Na2WO4.2H2O) at temperatures below 5oC. A heat treatment at temperatures at or above 300oC resulted in a phase transformation to monoclinic WO3, while preserving the nanoparticles morphology. The products were characterized using powder x-ray diffraction, transmission electron microscopy (including electron energy-loss spectroscopy and electron diffraction) and x-ray photoelectron spectroscopy., Comment: 11 pages, 1 table and 5 figures

EFhd2 is a conserved calcium-binding protein, abundant within the central nervous system. Previous studies identified EFhd2 associated with pathological forms of tau proteins in the tauopathy mouse model JNPL3, which expresses the human tau(P301L) mutant. This association was validated in human tauopathies, such as Alzheimer's disease (AD). However, the role that EFhd2 may play in tauopathies is still unknown. Here, we show that EFhd2 formed amyloid structures in vitro, a capability that is reduced by calcium ions. Electron microscopy (EM) analyses demonstrated that recombinant EFhd2 formed filamentous structures. EM analyses of sarkosyl-insoluble fractions derived from human AD brains also indicated that EFhd2 co-localizes with aggregated tau proteins and formed granular structures. Immunohistological analyses of brain slices demonstrated that EFhd2 co-localizes with pathological tau proteins in AD brains, confirming the co-aggregation of EFhd2 and pathological tau. Furthermore, EFhd2's coiled-coil domain mediated its self-oligomerization in vitro and its association with tau proteins in JNPL3 mouse brain extracts. The results demonstrate that EFhd2 is a novel amyloid protein associated with pathological tau proteins in AD brain and that calcium binding may regulate the formation of EFhd2's amyloid structures. Hence, EFhd2 may play an important role in the pathobiology of tau-mediated neurodegeneration.

An environmentally benign method capable of producing large quantities of materials was used to synthesize tungstite (WO3.H2O) leaf-shaped nanoplatelets (LNPs) and nanoribbons (NRs). These materials were simply obtained by aging of colloidal solutions prepared by adding hydrochloric acid (HCl) to dilute sodium tungstate solutions (Na2WO4.2H2O) at a temperature of 5-10oC. The aging medium and the pH of the precursor solutions were also investigated. Crystallization and growth occurred by Ostwald ripening during the aging of the colloidal solutions at ambient temperature for 24 to 48hrs. When dispersed in water, the LNPs and NRs take many days to settle, which is a clear advantage for some applications (e.g., photocatalysis). The materials were characterized using scanning and transmission electron microscopy, Raman and UV/Vis spectroscopies. The current versus voltage characteristics of the tungstite NRs showed that the material behaved as a Schottky diode with a breakdown electric field of 3.0x105V.m-1. They can also be heat treated at relatively low temperatures (300oC) to form tungsten oxide (WO3) NRs and be used as photoanodes for photoelectrochemical water splitting., Comment: 12 pages, 5 figures

We report on the temperature dependence of in-plane E2g and out of plane A1g Raman modes in high quality few layers MoS2 (FLMS) prepared using a high temperature vapor-phase method. The materials obtained were investigated using transmission electron microscopy. The frequencies of these two phonon modes were found to vary linearly with temperature. The first order temperature coefficients for E2g and A1g modes were found to be 1.32*10-2 and 1.23*10-2 cm-1/K, respectively. The thermal conductivity of the suspended FLMS at room temperature was estimated to be about 52 W/mK.

Candle wax was used as a precursor for the production of a diamond-nanotube composite in a single step. The composite films were fabricated by sulfur-assisted hot-filament chemical vapor deposition technique. The morphology of the composite films was analyzed by scanning electron microscopy and transmission electron microscopy. Raman spectra of the films show characteristic diamond band at 1,332 cm-1, D-band around 1,342 cm-1, and graphitic G-band around 1,582 cm-1. The electron energy-loss spectroscopy recorded at the carbon K-edge region shows signature features of diamond and carbon nanotube in the fabricated material. The ability to synthesize diamond-nanotube composites at relatively low temperatures by a single-step process opens up new possibilities for the fabrication of nanoelectronic devices.

The transformation of ≤4 nm equiatomic FePt nanoparticles from the disordered cubic A1 to the ordered tetragonal L10 phase was studied by means of high-resolution transmission electron microscopy coupled with in situ heating experiments. In accordance with ex situ annealing experiments, a transition temperature of around 500 °C was determined. Diffusion is enhanced at surfaces and plays a dominant role in the ordering process. Hence, the ordering of the crystallographic structure starts at the surface of the nanoparticles and propagates toward their center, resulting in complete ordering within some minutes, for temperatures above 600 °C. Unlike the generally assumed lower limit of ordering (3.5 nm), we demonstrate that ultrasmall (less than 3 nm) FePt nanoparticles can also be fully transformed to the L10 phase. The well-controlled and precise stoichiometry (Fe50 at.%Pt50 at.%) and the homogeneous composition of these particles both play a major role in their successful phase transformation.

Semiconductor quantum dots are considered very promising candidates for bio-imaging and diagnosis applications because of their tunable optical properties and good optical stability in aqueous phase. Any practical application of these materials will rely on the viability of their simple and direct synthesis in aqueous phase with no need for toxic and unstable organic media. The optical properties of CdSe quantum dots and CuS nanoparticles are desirable in bio-imaging and cell sorting applications because of their tunable photoluminescence at the visible range. The present work addresses the synthesis of CdSe quantum dots and CuS nanoparticles via an optimized, simple and scalable aqueous processing route at low temperatures. The tunability of the optical properties was achieved by a suitable control of the citrate/Cd mole ratio, temperature of synthesis (20-90°C) and reaction time (0-1 hour). In the case of CuS, the strong plasmonic absorption offers the opportunity to investigate this material as a photothermal coupling agent for photothermal therapy. The intensity of the plasmonic absorption was enhanced by selecting an appropriate sulfide precursor (Na2S, Thioglycolic acid), temperature of synthesis (90-120°C) and reaction time. Nanocrystals were characterized by x-ray diffraction, UV-VIS, photoluminescence (PL) spectroscopy techniques and electron microscopy. The effects of the synthesis conditions on the crystal size and the corresponding functional properties of synthesized quantum dots are presented and discussed.

Extended abstract of a paper presented at Microscopy and Microanalysis 2011 in Nashville, Tennessee, USA, August 7–August 11, 2011.

A systematic study was carried out to determine the effects of composition and grain size on the structural, optical and magnetic properties of pure ZnO and vanadium-doped ZnO nanocrystalline powders and films in the 0.0 at.% V - 6 at.% V range. The powders and films were synthesized via a sol-gel approach, where ethanolamine was used to increase the viscosity of the precursor solutions and promote the adhesion of the films onto quartz substrates. Powder X-ray diffraction confirmed the formation of ZnO (host oxide) after annealing of the precursors in air. The average grain size in the thin films ranged from 11 nm to 23 nm when the samples were annealed in air for one hour between 450ºC and 550ºC. UV-vis and photoluminescence confirmed the formation of the host oxide. Also, the photoluminescence intensity was found to be strongly dependent on the amount vanadium. Furthermore, it was found that the vanadium concentration and the annealing temperature play an important role in the ferromagnetic behavior of the material.

This study reports on the structural and magnetic characterizations of free-standing bismuth ferrite, BiFeO3, nanoparticles synthesized in polyol medium. Fine tuning of the ferrite magnetic properties was achieved by adding an excess bismuth species or doping with cobalt ions, coupled with thermal annealing. Crystalline Bi1-yCoyFeO3 powders (where ‘y’ ranges from 0.00 to 0.10) were produced after annealing the precursors for one hour at 700οC. The average crystallite size was calculated to be approximately 22 nm. We found that the synthesis under stoichiometric excess of Bi species (up to 10 at.%) promoted a more complete crystallization of the material, i.e., no precursor phases remained. Furthermore, both the saturation magnetization and the coercivity of the synthesized powders were strongly influenced by the concentration of Co. They increased from 0.13 emu/g and 19 Oe to 3.5 emu/g and 1183 Oe for pure BiFeO3 and 10 at.% Co-doped BiFeO3, respectively.

Carbon supported Au–Pt catalysts with different bimetallic compositions were prepared by water-in-oil (w/o) micro-emulsions. Carbon Vulcan XC-72R was added during the synthesis of particles in order to obtain good dispersion. Structural characterization was performed using XRD (X-ray diffraction) at wide angles, WAXS (wide-angle X-ray scattering) which showed that Pt–Au particles exhibited alloy properties in samples with high gold-content, and a segregation effect for those with low gold-content. Electrochemical characterization allowed estimation of the surface composition of Pt–Au alloys. These experiments have been confirmed by XRD data. Moreover, HRTEM (high resolution transmission electron microscopy) and XEDS (X-ray energy dispersive spectroscopy) characterization further confirmed the electrochemical results and XRD data. CO stripping experiments have shown an increasing bonding energy between CO and platinum with the gold content in the nanoalloys.

The response of solid to shock compression has been an interesting topic for more than a century. The present work is the first attempt to experimentally show that plastic deformation can be generated in brittle materials by a heat-assisted laser shock peening process, using silicon crystal as a sample material. Strong dislocation activity and large compressive residual stress are induced by this process. The dislocation structure is characterized with transmission electron microscopy and electron backscattered diffraction. The residual stress is measured using Raman scattering. This work presents a fundamental base for the application of laser shock peening in brittle materials to generate large compressive residual stress and plastic deformation for better mechanical properties, such as fatigue life and fracture toughness.

Extended abstract of a paper presented at Microscopy and Microanalysis 2013 in Indianapolis, Indiana, USA, August 4 – August 8, 2013.

Electronic devices based on single crystal SiC represent a good choice for a variety of new high temperature, high power electronics applications. The challenge is to develop a package that is resistant to thermal degradation in harsh environments. Conditions are extreme and this all but rules out only a handful of materials and materials systems. Polycrystalline SiC is the material that we have chosen to study as a suitable package and materials suitability/compatibility has been considered on several levels.

Extended abstract of a paper presented at Microscopy and Microanalysis 2012 in Phoenix, Arizona, USA, July 29 – August 2, 2012.

Extended abstract of a paper presented at Microscopy and Microanalysis 2012 in Phoenix, Arizona, USA, July 29 – August 2, 2012.

Extended abstract of a paper presented at Microscopy and Microanalysis 2012 in Phoenix, Arizona, USA, July 29 – August 2, 2012.