We present a spectroscopic and microscopic study of nanoscale Al and Si films electrodeposited in water- and air-stable ionic liquids. The choice of cations for such ionic liquids has previously been shown to have a significant effect on the crystallite size of electrodeposited Al or Si films. We found that the deposits are generally uniform, dense, metallic bright, and adherent with crystallite sizes in the nanometer range. The nanocrystalline films were characterized using X-ray Photoelectron Spectroscopy (XPS) and High-Resolution Scanning Electron Microscopy (HRSEM). The XPS results show that the surface of both films is oxidized although the deposition was done in an inert gas glove box. Furthermore our results suggest that as a consequence of oxygen attack the nanoparticles are composed of a metallic core surrounded by a thin oxidic shell. Our XPS study also shows that neither the cation nor the anion of the ionic liquid is entrapped in the deposit. Thus, electrodeposition in ionic liquids delivers pure materials.
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