C. López-Cartes

Atomic-scale imaging of carbon nanofibre growth

The synthesis of carbon nanotubes with predefined structure and functionality plays a central role in the field of nanotechnology, whereas the inhibition of carbon growth is needed to prevent a breakdown of industrial catalysts for hydrogen and synthesis gas production. The growth of carbon nanotubes and nanofibres has therefore been widely studied. Recent advances in in situ techniques now open up the possibility of studying gas–solid interactions at the atomic level. Here we present time-resolved, high-resolution in situ transmission electron microscope observations of the formation of carbon nanofibres from methane decomposition over supported nickel nanocrystals. Carbon nanofibres are observed to develop through a reaction-induced reshaping of the nickel nanocrystals. Specifically, the nucleation and growth of graphene layers are found to be assisted by a dynamic formation and restructuring of mono-atomic step edges at the nickel surface. Density-functional theory calculations indicate that the observations are consistent with a growth mechanism involving surface diffusion of carbon and nickel atoms. The finding that metallic step edges act as spatiotemporal dynamic growth sites may be important for understanding other types of catalytic reactions and nanomaterial syntheses.

Mechanical behavior and oxidation resistance of Cr(Al)N coatings

Nanocrystalline chromium nitride and ternary chromium aluminium nitride thin films were deposited by reactive magnetron sputtering of Cr and Al targets in argon/nitrogen atmosphere varying the sputtering power and gas composition. The coatings were characterized in terms of crystal phase, chemical composition, microstructure, and mechanical properties by x-ray diffraction, x-ray photoelectron spectroscopy, including x-ray-induced Auger electron spectroscopy, transmission electron microscopy, selected-area electron diffraction, electron energy-loss spectroscopy, cross-sectional scanning electron microscopy, and ultramicrohardness tester. The incorporation of Al in the composition of the films produces an increase in the mechanical properties (hardness and reduced Young’s modulus) and an increased thermal resistance against oxidation in comparison to the pure CrN composition. The hardness behavior was attributed mainly to a reduction of the CrN crystallite size according to a Hall–Petch relationship. The ox...

Structural characterisation of a VMgO catalyst used in the oxidative dehydrogenation of propane

AbstractA VMgO catalyst (containing 14 wt% vanadium) that is used in the oxidative dehydrogenation of propane (ODHP) reaction has been examined in detail by in situ EXAFS, in situ XRD and HREM. These characterisation techniques have revealed that, as prepared, the catalyst is in effect a three-component system comprising discrete magnesium orthovanadate (Mg3V2O8) particles, magnesium oxide and a disordered vanadium-containing overlayer supported on the MgO. When the catalyst is exposed to typical ODHP reaction conditions at

Structure of highly dispersed metals and oxides: exploring the capabilities of high‐resolution electron microscopy

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In situ transmission electron microscopy investigation of Ce(IV) and Pr(IV) reducibility in a Rh (1%)/Ce0.8Pr0.2O2−x catalyst

the in situ EXAFS indicates a change in vanadium oxidation state from 5+ to 3+. Under the same conditions, in situ XRD suggests that Mg3V2O8 transforms to a cubic spinel type structure with a lattice parameter of 8.42 Å. These changes are reversible on exposure to air at

Contribution of electron microscopy techniques to the chemical and structural characterization of TiC/a-C nanocomposite coatings

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