A Descriptive in vitro Electron Microscopic Study of Acidic Fluoride-Treated Enamel: Potential Anti-Erosion Effects

This study aimed to investigate the surface zones of acidic fluoride-treated enamel. Human teeth were each divided into three or four enamel specimens that were treated for 10 min with solutions of 0.2 and 0.4% HF (pH 3.09 and 2.94), 1.74% SnF2 (pH 2.9), 0.68% TiF4 (pH 1.6) and 0.84% NaF (pH 4.5). Untreated specimens functioned as negative controls. The microstructure and elemental composition of the surface zones were studied by scanning electron microscopy/energy-dispersive X-ray (EDX) analysis, transmission electron microscopy (TEM) and nanospot-EDX following cross-sectional preparation using focused ion beam technology. TEM/EDX analyses of NaF-treated specimens showed a 500-nm-thick closed surface film containing 20-40 at% (atomic percent) F. HF-treated specimens had a distinct surface film 200-600 nm thick (dense, not globular) containing 45-47 at% F. TiF4-treated specimens had a surface film of 200-300 nm in thickness containing 8-11 at% Ti but no detectable fluoride. SnF2-treated specimens had a modified surface enamel layer varying in thickness from 200 to 800 nm with an inhomogeneous distribution of Sn. Local spots were detected with as high as 8 at% Sn (30 wt%, weight percent). The results suggest that the reaction mechanisms of SnF2 and TiF4 solutions with dental enamel differ from those occurring after enamel exposure to acidulated NaF and HF solutions. While the HF and NaF treatments resulted in the formation of CaF2-like material as shown by EDX, no significant surface fluoridation was found for SnF2 and TiF4 solutions within the TEM/EDX detection limits. These results suggest that the erosion-protective mechanisms of these latter compounds probably relate more to the formation of hardly soluble and acid-resistant reaction surface films and less to surface fluoride incorporation.