Hjortsjö Carl, Young Alix, Kiesow Andreas, Cismak Andreas, Berthold Lutz, Petzold Matthias
Department of Prosthetic Dentistry and Oral Function, Institute of Clinical Dentistry, Faculty of Dentistry, University of Oslo, Oslo, Norway.
Caries Res. 2015;49(6):618-25. doi: 10.1159/000441195. Epub 2015 Nov 5.
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.
本研究旨在调查经酸性氟化物处理的牙釉质的表面区域。将人类牙齿分别切成三或四个牙釉质样本,用0.2%和0.4%的HF(pH 3.09和2.94)、1.74%的SnF₂(pH 2.9)、0.68%的TiF₄(pH 1.6)和0.84%的NaF(pH 4.5)溶液处理10分钟。未处理的样本用作阴性对照。使用聚焦离子束技术进行横截面制备后,通过扫描电子显微镜/能量色散X射线(EDX)分析、透射电子显微镜(TEM)和纳米点EDX研究表面区域的微观结构和元素组成。对经NaF处理的样本进行的TEM/EDX分析显示,有一层500纳米厚的封闭表面膜,含20 - 40原子百分比的F。经HF处理的样本有一层明显的表面膜,厚度为200 - 600纳米(致密,非球状),含45 - 47原子百分比的F。经TiF₄处理的样本有一层厚度为200 - 300纳米的表面膜,含8 - 11原子百分比的Ti,但未检测到氟化物。经SnF₂处理的样本有一层厚度从200到800纳米不等的改性表面牙釉质层,Sn分布不均匀。局部斑点检测到的Sn含量高达8原子百分比(30重量百分比)。结果表明,SnF₂和TiF₄溶液与牙釉质的反应机制不同于牙釉质暴露于酸化NaF和HF溶液后的反应机制。虽然EDX显示HF和NaF处理导致形成了类似CaF₂的物质,但在TEM/EDX检测限内,未发现SnF₂和TiF₄溶液有明显的表面氟化现象。这些结果表明,后两种化合物的防侵蚀机制可能更多地与形成难溶性和耐酸反应表面膜有关,而与表面氟化物掺入关系较小。