RESUMO
Nanoscale bimetallic Pd-Ti catalysts on carbon supports were prepared in liquid using ammonium tetrachloropalladate and titanium isopropoxide. The size of the metal particles ranged from subnanometer to greater than 10 nm, and the X-ray diffraction pattern of metal particles was dominated by a cubic crystalline structure. Depending upon the preparation conditions, the catalysts were comprised of Pd and TiO2 or Pd3Ti-like alloy. The surface Ti/Pd ratio was much greater than the original metal loading. We propose that the bimetallic particles were comprised of short-range Pd and TiO2 or Pd-Ti alloy nanocrystal covered by a thin TiO2 layer.
RESUMO
A new constant-distance imaging method based on the relationship between tip impedance and tip-substrate separation has been developed for the scanning electrochemical microscope. The tip impedance is monitored by application of a high-frequency ac voltage bias between the tip and auxiliary electrode. The high-frequency ac current is easily separated from the dc-level faradaic electrochemistry with a simple RC filter, which allows impedance measurements during feedback or generation/collection experiments. By employing a piezo-based feedback controller, we are able to maintain the impedance at a constant value and, thus, maintain a constant tip-substrate separation. Application of the method to feedback and generation/collection experiments with tip electrodes as small as 2 microm is presented.