Abstract
Preparation of thin U- and Th-coated 0.3mm diameter Pt working electrodes by the cyclic potential sweep method is described. Uranyl- and thorium hydroxide layers were electrodeposited from ethanol solutions containing 0.02M natural uranyl and 0.02M natural thorium nitrate, each with 3.6M ammonium nitrate. The cell for electrodeposition was specially developed in order to accommodate the small working electrodes for this research by including a working electrode probe, 3-D translation stage, and microscope. The source material deposition was analyzed using digital microscopy and scanning electron microscopy, and confirmed using x-ray fluorescence measurements. The appropriate potential range for electrodeposition was determined to be −0.62V to −0.64V for a 0.3mm diameter Pt working electrode placed 1cm from the counter electrode. Smooth, uniform deposition was observed near the central region of the working electrode, while surface cracking and crystalline formations were found near the edge of the working electrode. The final procedure for sample substrate preparation, electrolytic solution preparation and electrodeposition are described.
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