In order to monitor the degradation level at the alloy-electrocatalysts during the anodic polarization under N2 atmosphere in h3po4 electrolyte at elevated temperatures, a specially designed cell was prepared (see Fig. l).The cell had a window covered with a polyimide film for X-ray diffraction. The electrocatalyst used was Pl-Co-Ni alloy(ca.2/l/l gross atomic ratio),supported on carbon black(CB). The alloy-electrocatalysts loading on CB was 20 weight

Polyimide film Insulation sheet Carbon paper Sample catalyst —

(H3P0„) PTFE sheet Matrix H2 electrode Carbon holder

X-ray diffractometer

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