Microanalysis of Palladium after Electrolysis in Heavy Water

The morphology and microcomposition of palladium after electrolysis in heavy water were studied. Fibers which appeared on the surface were observed to change with time. Evidence which supports the possibility of transmutation is presented. INTRODUCTION Previously we reported finding concentrations of unexpected elements on palladium cathodes after electrolysis in an electrolyte containing H2SO4 and D2O (1,2). We report here the results of analysis of palladium 0.315 mm thick used as a cathode for 25 hours and then inadvertently as an anode for 170 minutes. EXPERIMENTAL METHODS AND RESULTS The electrolysis experiments have been carried out, first, for about 5 hours during summer 1993, and then for about 23 hours during summer 1994. For the first 5 hours of operation, the experimental setup consisted of two cells in series, one (light water control cell) containing 0.06 mol fraction H2SO4 (analytical reagent) in deionized H2O, the other (heavy water cell) contained 0.06 mol fraction H2SO4 in D2O (99% D2) and both containing a cold-rolled Pd cathode and a Pt anode. The anodes were made from 99.9% platinum and the cathodes were made from 99.9% palladium. Chemical analyses of the palladium and platinum were provided by the supplier. The palladium foils were produced by cold rolling from the initial 0.5 mm thickness to 0.315 mm. For the next 20 hours of operation, a new setup was used. Two cells were connected in series but, this time, the control cell contained two Pt electrodes, and the experimental cell contained the previous Pd cathode and Pt anode of the heavy water cell. Both contained acidified heavy water (0.06 mol fraction H2SO4 ). In the last experiment, the palladium was used inadvertently as an anode. After electrolysis for 170 minutes, the cell current rapidly dropped to zero. When the cell was opened, we found that the lower part of the palladium had dissolved. The electrolyte, originally a clear liquid, was now a black powdery solid. Some of this black solid was attached to the platinum anode but the platinum was not damaged. In this series of experiments, a recombination catalyst consisting of a substrate coated with platinum black (Los Alamos type electrode, 20% Pt on carbon) was utilized to recombine the off-gases in a closed system. Electrolysis was performed at current densities ranging from 0.75 to 1.5 A per cm. Dash, J. and S. Miguet, Microanalysis of Pd Cathodes after Electrolysis in Aqueous Acids. J. New Energy, 1996. 1(1): p. 23.