Sm 09020 cp

A tooth extracted because of periodontal pathology (approved by the Commission for Medical Ethics of Okayama University Hospital under file number 1901-036) was collected. The tooth was adhesively restored 9 years ago using Clearfil SE Bond ('C-SE' as pre-cursor of C-SE2; Kuraray Noritake) and the resin-based composite Clearfil AP-X (Kuraray Noritake). The tooth was fixed in glutaraldehyde, gradually dehydrated in ethanol and embedded in epoxy resin. After the adhesive-dentin interface was exposed, the interface was mechanically polished using diamond lapping film (3M, St. Louis, MO, USA), followed by broad argon-ion-beam polishing using a crosssection polisher (SM-09020 CP, JEOL). Subsequently, a thin layer of carbon was deposited on the surface (JEE-420T, JEOL), upon which the specimens were examined with Feg-SEM (JSM-6701F, JEOL) operated at 5 kV and employing an annular semiconductor detector. For TEM, ultrathin sections were cut (Leica EM UC7, Leica, Vienna, Austria), prior to being examined with highresolution 200-kV TEM utilizing a JEM-2100 (JEOL) microscope.

SEM (SU-70, Hitachi High-Technologies Co., Tokyo, Japan, and JCM-5700, JEOL, Tokyo, Japan) was used to observe the microstructure of the HApS particles and the fractured surface (after flexural strength measurement) of the set cement. For SEM observations, the specimens were sputter coated with osmium. Moreover, crosssectional SEM specimens were prepared using a crosssection polisher (SM-09020CP, JEOL) and backscatter electron imaging was performed in a field-emission SEM system (JSM-6701F, JEOL, Tokyo, Japan). Elemental analysis was carried out for the original HApS particles, the glass cores, and the matrix in the GIC-S and AIC-S specimens, and for HApS inside the AIC-S specimens using an EDS detector (IncaPentaFETx3, Oxford Instruments PLC., Oxford, UK) and SEM (SU-70, Hitachi High-Technologies Co., Tokyo, Japan). The pressure voltmeter was set at 20 kV for 300 s.