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We investigated the reduction mechanism of surface oxide on aluminum alloy powders containing magnesium, by x-ray photoelectron spectroscopy using synchrotron radiation (SR-XPS). The reduction is the initial reaction in a new aluminum nitridation method developed by one of the authors. In heating the powders to 823 K, magnesium soluted in the powders moves from the inner region to the surface at temperatures below 573 K, and finally, above 773 K, the magnesium reduces the aluminum oxide of powder surfaces by chemical reaction, which breaks the surface oxide films, and metallic aluminum appears on the topmost surface of the powders. These results suggest that the SR-XPS system is very useful for dynamic chemical reaction analysis of the surface via in situ measurement. © 1997 American Institute of Physics.