The analysis of sulfur distribution in porous carbon/sulfur nanocomposites using small-angle X-ray scattering (SAXS) is presented. Ordered porous CMK-8 carbon was used as the host matrix and gradually filled with sulfur (20-50 wt %) via melt impregnation. Owing to the almost complete match between the electron densities of carbon and sulfur, the porous nanocomposites present in essence a two-phase system and the filling of the host material can be precisely followed by this method. The absolute scattering intensities normalized per unit of mass were corrected accounting for the scattering contribution of the turbostratic microstructure of carbon and amorphous sulfur. The analysis using the Porod parameter and the chord-length distribution (CLD) approach determined the specific surface areas and filling mechanism of the nanocomposite materials, respectively. Thus, SAXS provides comprehensive characterization of the sulfur distribution in porous carbon and valuable information for a deeper understanding of cathode materials of lithium-sulfur batteries.
The photoisomerization properties of an azobenzene derivative on a thin insulating NaCl layer on Ag(111) are investigated with a low-temperature scanning tunneling microscope and density functional calculations. Illumination with UV light at 365 nm induces the reversible direct isomerization of the adsorbed species, while visible light does not lead to any changes. This unexpected behavior cannot be explained by the change of the electronic structure upon adsorption on the inert surface. It is rationalized in terms of electrostatic interactions caused by the atomistic details of the surface.
SummaryHollow carbon spheres (HCS) with a nanoporous shell are promising for the use in lithium–sulfur batteries because of the large internal void offering space for sulfur and polysulfide storage and confinement. However, there is an ongoing discussion whether the cavity is accessible for sulfur. Yet no valid proof of cavity filling has been presented, mostly due to application of unsuitable high-vacuum methods for the analysis of sulfur distribution. Here we describe the distribution of sulfur in hollow carbon spheres by powder X-ray diffraction and Raman spectroscopy along with results from scanning electron microscopy and nitrogen physisorption. The results of these methods lead to the conclusion that the cavity is not accessible for sulfur infiltration. Nevertheless, HCS/sulfur composite cathodes with areal sulfur loadings of 2.0 mg·cm−2 were investigated electrochemically, showing stable cycling performance with specific capacities of about 500 mAh·g−1 based on the mass of sulfur over 500 cycles.
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