The deposition of metal contaminants (e.g., Ni, V, and Fe) from the hydrocarbon feed causes the deactivation of fluid catalytic cracking (FCC) catalyst used in petroleum refining. It is very important to understand the changes in the morphology and chemical composition on the catalyst surface and how these structural and chemical changes affect the catalyst performance. In this research, metal-contaminated FCC catalysts from a commercial unit have been characterized using AFM together with SEM - EDS. The AFM images showed the surface pores as well as the features that surround the pore's entrance on the catalyst surface. Catalyst surface contains debris that appear as bright spots in AFM images. SEM - EDS results have shown the presence of iron in these bright spots. Fe enrichment at the catalyst particle surface was also confirmed by XPS analyses.