The reduction and electrodeposition of TcO4- on a smooth gold foil electrode with an exposed area of 0.25 cm(2) was performed in 1 M H2SO4 supporting electrolyte using bulk electrolysis with a constant current density of 1.0 A/cm(2) at a potential of -2.0 V. Significant hydrogen evolution accompanied the formation of Tc deposits. Tc concentrations consisted of 0.01 M and 2 x 10(-3) M and were electrodeposited over various times. Deposited fractions of Tc were characterized by powder x-ray diffraction, x-ray absorption fine structure spectroscopy, and scanning electron microscopy with the capability to measure semiquantitative elemental compositions by energy-dispersive x-ray emission spectroscopy. Results indicate the presence of Tc metal on all samples as the primary electrodeposited constituent for all deposition times and Tc concentrations. Thin films of Tc have been observed followed by the formation of beads that are removable by scratching. After 2000, the quantity of Tc removed from solution and deposited was 0.64 mg Tc per cm(2). The solution, after electrodeposition, showed characteristic absorbances near 500 nm corresponding to hydrolyzed Tc(IV) produced during deposition of Tc metal. No detectable Tc(IV) was deposited to the cathode. (C) 2011 The Electrochemical Society. [DOI: 10.1149/1.3533364] All rights reserved.