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Completed in 2007, this work is a PhD thesis that presents measurements of the stability and activities of Pt-based oxygen reduction reaction electrocatalysts for proton exchange membrane fuelcells using a combinatorial materials synthesis approach developed at Dalhousie University. Numerous combinatorial libraries of Pt1-xMx (M = Fe, Ni, Mn)and Pt1-x-yMxMy (M, M = Co, Ni, Mn, Fe) were prepared by magnetron sputtering using 3M sproprietary nano-structured thin film supports as substrates. The composition of these libraries after acid treatment was very close to the electrocatalysts tested in hydrogen fuel cells, thus showing that acid treatment can effectively mimic the fuel cell environment. Detailed studies of the ORR activity of sputtered Pt1-xCox films, using rotating ring-disk electrode (RRDE) techniques, importance of bench line measurements and the impact of catalyst loadings in RRDE measurements are also discussed.