The pulsed bipolar electrodeposition of palladium onto 1-2 mum graphite par
ticles was investigated. The amount of palladium deposited was strongly cor
related with field intensity, showing an abrupt increase at 2-3 kV/cm. The
electrodeposition was successful for frequencies ranging from 500 Hz to 20
kHz, and the amount of deposited palladium was independent of the frequency
used. These results demonstrate that the preparation of bipolar electrodep
osited catalysts can be achieved within a very large frequency window. Pall
adium surface area measurements indicate an increase in dispersion with inc
reasing frequency. Sonication of the graphite prior to deposition leads to
significantly greater palladium dispersion. Electron microscopy characteriz
ation reveals three types of growth: surface-bound, ramified, and amorphous
. The surface-bound growth appears as spherical deposits on the order of 5
nm in both do and pulsed-field experiments. The ramified deposits consist o
f interconnected 25-50 nm diam spherical structures extending from the grap
hite particles and appear in the samples prepared at all studied frequencie
s. (C) 2001 The Electrochemical Society.