Rodrigo Esparza

Experimental evidence of icosahedral and decahedral packing in one-dimensional nanostructures.

The packing of spheres is a subject that has drawn the attention of mathematicians and philosophers for centuries and that currently attracts the interest of the scientific community in several fields. At the nanoscale, the packing of atoms affects the chemical and structural properties of the material and, hence, its potential applications. This report describes the experimental formation of 5-fold nanostructures by the packing of interpenetrated icosahedral and decahedral units. These nanowires, formed by the reaction of a mixture of metal salts (Au and Ag) in the presence of oleylamine, are obtained when the chemical composition is specifically Ag/Au = 3:1. The experimental images of the icosahedral nanowires have a high likelihood with simulated electron micrographs of structures formed by two or three Boerdijk-Coxeter-Bernal helices roped on a single structure, whereas for the decahedral wires, simulations using a model of adjacent decahedra match the experimental structures. To our knowledge, this is the first report of the synthesis of nanowires formed by the packing of structures with 5-fold symmetry. These icosahedral nanowire structures are similar to those of quasicrystals, which can only be formed if at least two atomic species are present and in which icosahedral and decahedral packing has been found for bulk crystals.

On the behavior of Ag nanowires under high temperature: in situ characterization by aberration-corrected STEM

Single crystal nanowires have been monitored at a wide range of temperatures from room temperature up to 900 °C using an aberration-corrected JEOL 2200FS scanning transmission electron microscope in both, bright field and high angle annular dark field, modes. The in situ measurements allowed heating and cooling the material instantaneously at the desired value making able to analyze the behaviour of silver nanowires at atomic resolution. The nanowires which firstly melted and subsequently vaporized left after the reaction empty carbon nanotubes. In addition, a Chevron-like defect has been also observed for the first time in silver nanowires and a structural analysis has been carried out by aberration corrected scanning transmission electron microscopy using high angle annular dark field imaging.

A synthesis route of gold nanoparticles without using a reducing agent

In the present work we show that synthesis of gold nanoparticles (NPs) could be performed by microwave-assisted technique without the need of adding any reducing agent. Only water and the gold salt precursor are necessary to generate the NPs under the influence of microwaves. The produced NPs have been characterized by state-of-art microscopy techniques, like high resolution transmission electron microscopy, scanning electron microscopy, and energy-dispersive x-ray. Theoretical calculations have been performed to support the experimental findings. It is expected that the present work opens routes for synthesis of NPs using green, fast, and safe methods.

Analysis of electron beam damage of exfoliated MoS2 sheets and quantitative HAADF-STEM imaging

In this work we examined MoS₂ sheets by aberration-corrected scanning transmission electron microscopy (STEM) at three different energies: 80, 120 and 200 kV. Structural damage of the MoS₂ sheets has been controlled at 80 kV according a theoretical calculation based on the inelastic scattering of the electrons involved in the interaction electron-matter. The threshold energy for the MoS₂ material has been found and experimentally verified in the microscope. At energies higher than the energy threshold we show surface and edge defects produced by the electron beam irradiation. Quantitative analysis at atomic level in the images obtained at 80 kV has been performed using the experimental images and via STEM simulations using SICSTEM software to determine the exact number of MoS2₂ layers.

In situ TEM study of mechanical behaviour of twinned nanoparticles

There is strong interest in studying changes in mechanical properties with reducing grain size. The rational is that consequent dislocation glide cannot be sustained, resulting in an increase in material strength. However, this comes with the cost of a reduction in ductility. It has been shown that coherent twin boundaries in nanostructured Cu improve the ductility to 14% [Lu et al., Science 324 (2009) p. 349]. In this paper, we report for the first time the compression of individual nanoparticles using an in situ force probing holder in the transmission electron microscope. Four types of nanoparticles were tested, three with twin boundaries (decahedra, icosahedra and a single twin) and one free of defects (octahedral). Our results indicate the yield strength of the twinned nanoparticles is between 0.5 and 2.0 GPa. The total malleability for the twinned particles range from 80 to 100%. In addition, experimental results were reproduced by MD simulations of the compression phenomena and suggest that the outstanding mechanical properties are related with partial dislocation multiplication at twin boundaries.

Pb(core)/ZnO(shell) nanowires obtained by microwave-assisted method

In this study, Pb-filled ZnO nanowires [Pb(core)/ZnO(shell)] were synthesized by a simple and novel one-step vapor transport and condensation method by microwave-assisted decomposition of zinc ferrite. The synthesis was performed using a conventional oven at 1000 W and 5 min of treatment. After synthesis, a spongy white cotton-like material was obtained in the condensation zone of the reaction system. HRTEM analysis revealed that product consists of a Pb-(core) with (fcc) cubic structure that preferentially grows in the [111] direction and a hexagonal wurtzite ZnO-(Shell) that grows in the [001] direction. Nanowire length was more than 5 μm and a statistical analysis determined that the shell and core diameters were 21.00 ± 3.00 and 4.00 ± 1.00 nm, respectively. Experimental, structural details, and synthesis mechanism are discussed in this study.

Atomic Surface Segregation and Structural Characterization of PdPt Bimetallic Nanoparticles

Bimetallic nanoparticles are of interest since they lead to many interesting electrical, chemical, catalytic, and optical properties. They are particularly important in the field of catalysis since they show superior catalytic properties than their monometallic counterparts. The structures of bimetallic nanoparticles depend mainly on the synthesis conditions and the miscibility of the two components. In this work, PdPt alloyed-bimetallic nanoparticles (NPs) were synthesized through the polyol method, and characterized using spherical aberration (Cs) corrected scanning transmission electron microscopy (STEM). High-angle annular dark-field (HAADF)-STEM images of bimetallic nanoparticles were obtained. The contrast of images shows that nanoparticles have an alloy structure with an average size of 8.2 nm. Together with the characterization of nanoparticles, a systematic molecular dynamics simulations study focused on the structural stability and atomic surface segregation trends in 923-atom PdPt alloyed-bimetallic NPs was carried out.

Insights into the structure of MoS2/WS2 nanomaterial catalysts as revealed by aberration corrected STEM

Molybdenum disulfide/Tungsten disulphide (MoS2/WS2) is a compound very useful for its properties; it is used as lubricant, catalyst in hydrodesulfuration, in hydrogen fuel storage, etc. As part of the 2nd Joint Congress of the Portuguese and Spanish Microscopy Societies the present work reports about the different types of MoS2/WS2 nanomaterials which have been investigated by using aberration corrected STEM namely: (1) MoS2 nanotubes (2) MoS2 hexagonal nanoplates, (3) rippled or helical MoS2 nanowires, (4) Co-doped MoS2/WS2 nanowires and (5) fullerene-like WS2 nanoparticles