Surface Characterization of Amalgams Using X-ray Photoelectron Spectroscopy

This study is the first to report on the use of x-ray photoelectron spectroscopy (XPS or ESCA) for studying the surface films (less than 10 nm thick) of aged amalgams. The concentrations and electron binding energies of the elements on the surfaces of four different amalgams aged for 20 min, one day, seven days, and 30 days were determined quantitatively. For comparison, the bulk compositions of the amalgams aged for seven days were also determined after removal of approximately 5 nm of material from the surface by argon-ion-sputtering. The XPS data revealed that the surface films of aged zinc-containing amalgams were not a simple oxide but were primarily composed of a (hydrated) tin and zinc oxy-hydroxide, whereas, in the zinc-free amalgams, the surface films were primarily a tin oxide. The concentration of mercury in this thin surface film after aging was depleted. This suggests that tin and/or zinc preferentially diffused to the surface and combined with oxygen, forming a surface film and diluting the mercury concentration in the surface. Another probable explanation for the depleted mercury is that a minimal amount of mercury in the surface film evaporated during the aging.