Complementary microscopy techniques applied for optimizing the structure and performance of graphene-based hybrids.

To improve the performance of graphene and to extend its potential applications, one of the most effective efforts is to hybridize graphene with one or more metal/metal oxide nanocrystals (NCs). In this paper, we demonstrate the complementary techniques of X-ray diffraction, high resolution electron microscopy (HREM), energy-dispersive X-ray spectroscopy (EDX), and energy-filtered transmission electron microscopy (EFTEM), which enables us to optimize the synthetic conditions, improve the quality of attached NCs, and tailor the performance of graphene-based hybrids for green energy related applications. Specifically, we explored the EFTEM technique to characterize two graphene-based composites. For the first sample of graphene/CoO(x), we present how the oxygen elemental map can identify that the oxidization of attached cobalt NCs most likely occurred during post treatments, rather than during the solvothermal reaction; for the second sample of graphene/(Mn, Co, Ni)O(x), we demonstrate how two-dimensional elemental mapping can differentiate the distribution of Mn, Co, and Ni on the surface of graphene. The results indicate that the EFTEM technique can supply very valuable and indispensable information, which contributes to comprehensive evaluation of structure and performance of graphene based hybrids.

One-step Melt Synthesis of Water Soluble, Photoluminescent, Surface-Oxidized Silicon Nanoparticles for Cellular Imaging Applications.

We have developed a versatile, one-step melt synthesis of water-soluble, highly emissive silicon nanoparticles using bi-functional, low-melting solids (such as glutaric acid) as reaction media. Characterization through transmission electron microscopy, selected area electron diffraction, X-ray photoelectron spectroscopy, and Raman spectroscopy shows that the one-step melt synthesis produces nanoscale Si cores surrounded by a silicon oxide shell. Analysis of the nanoparticle surface using FT-IR, zeta potential, and gel electrophoresis indicates that the bi-functional ligand used in the one-step synthesis is grafted onto the nanoparticle, which allows for tuning of the particle surface charge, solubility, and functionality. Photoluminescence spectra of the as-prepared glutaric acid-synthesized silicon nanoparticles show an intense blue-green emission with a short (ns) lifetime suitable for biological imaging. These nanoparticles are found to be stable in biological media and have been used to examine cellular uptake and distribution in live N2a cells.