The purpose of this study was to compare the amount of calcium fluoride deposited on the enamel and dentin surface and to obtain information on the morphological change and crystallographic details of mineral deposition after 12,000ppm APF application in vitro. The bovine enamel and dentin blocks were randomly assigned to eight groups according to artificial caries lesion formation and difference of fluoride application time. The fluoride concentration and morphological characteristics on the treated enamel and dentin surface were investigated by using fluoride quantitative analysis and SEM. The powdered enamel and dentin of the intact bovine incisors were prepared for the X-ray diffraction analysis. The following results were obtained. 1. The amounts of KOH-soluble fluoride on the carious enamel and dentin surface after 24h APF application were higher than after only 5min APF application(p<0.05), but in the case of the sound enamel and dentin surface were similar after 5min and 24h application (P>0.05). The fluoride content was highly increased in the carious dentin as compared with sound dentin after APF application(P<0.05). 2. The carious enamel surface after APF application, the demineralized enamel surface were recovered a more dense enamel surface and precipitation of crystal was observed a distintive surface layer of spherical globules of about 1 m diameter. In the case of the fluorided carious dentin surface, precipitation of calcium fluoride-like material was deposited both inside the dentinal tubules as well as in the intertubular regions. 3. The crystallographic structure of powdered enamel and dentin after 24h APF application had large crystallities of apatite and CaF2 diffraction peaks in the enamel as compared with dentin. The diffraction data collected from the 27.50-29.50(2) angular range of the powdered enamel, the (105) apatite, (225) apatite and (111) CaF2 peaks of the enamel crystallities were detected after 24h APF application.