The feature of the process for ultra-low alloy catalyst loading electrode according to this invention is to reduce its alloy formation period of aging process subsequent to hydrogen reduction process of catalyst ions after ion exchange process of proton for their ions in the cluster of the polymer electrolyte on the surface of the carbon powder. The process is able to drastically shorten the aging time with temperature rise beyond 200.degree. C. up to 400.degree. C. under hydrogen atmosphere for the formation of alloy catalyst, for example Pt--Ru binary by the additional processes of pre-treatment of substituting K.sup.+, Na.sup.+, Li.sup.+, Rb.sup.+, Cs.sup.+, Mg.sup.2+, Ca.sup.2+, Ba.sup.2+, Fe.sup.2+, Sr.sup.2+, Ra.sup.2+, Cu.sup.2+, Ag.sup.+, Zn.sup.2+, Ni.sup.2+, or Co.sup.2+ for proton before the hydrogen reduction process. The further post-treatment of substituting K.sup.+, Na.sup.+, Li.sup.+, Rb.sup.+, Cs.sup.+, Mg.sup.2+, Ca.sup.2+, Ba.sup.2+, Fe.sup.2+, Sr.sup.2+, Ra.sup.2+, Cu.sup.2+, Ag.sup.+, Zn.sup.2+, Ni.sup.2+, or Co.sup.2+ for proton before the ion exchange process is more preferable. This new process is little harmful to the CO tolerance performance of PEFC.

 
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