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The aim of this study was to investigate the effects of potassium fluoride (KF) and sodium fluoride (NaF) in different concentrations on micro-shear bond strength (µSBS) and their protective effects against acid. The enamel blocks were treated with several concentrations of KF and NaF. For µSBS, Clearfil SE Bond 2 was applied to the treated surface and resin composite was light-cured, then examined using a universal testing machine. For acid resistance test, the specimens were immersed in acidic solution (pH 4.5), then examined under 3D confocal laser scanning microscope (CLSM). In µSBS, KF at 1,000, 9,000, and 10,000 ppm did not show differences compared with the control, while other concentrations of KF and NaF led to decreased µSBS. Higher concentrations of NaF and KF showed higher resistance to the acid challenge. So, we concluded that various concentrations of KF and NaF solutions had specific effects on µSBS and acid resistance.

We studied the phase stability of Ce-substituted magnetoplumbite-type Sr ferrite under various oxygen pressures. We have successfully obtained Ce-substituted samples as revealed from X-ray diffraction and wavelength dispersion X-ray analyses. The solubility limit of Ce in Sr1- x Ce x Fe12O19 was estimated to be $x = 0.24$ at ambient pressure, which is reduced to 0.05–0.10 under higher oxygen pressures. The variation of the $c$ -axis against $x$ and the reduction of the solubility by increasing oxygen pressure suggests that the valence of Ce is not 4+ but 3+. The solubility limit of Ce is dominated not only by the ionic radius but also by the valence instability of Ce.

The purpose of this study was to investigate the formation of acid-base resistant zone (ABRZ) of enamel surface during bracket bonding by using three self-etch adhesives presently available in the orthodontic treatment. Also, the relation between the thickness of the ABRZ and bonding strength, the relation between the thickness of the ABRZ and the concentration of fluoride ions contained in the adhesives, were discussed respectively. The ABRZ was formed with all self-etch orthodontic adhesives. ABRZ thicknesses of two self-etch adhesives were approximately 0.8-1.0 μm, whereas ABRZ thickness of other one was about 0.1 μm. The bond strengths of all self-etch orthodontic adhesives indicated over 10 MPa, and ABRZ thickness observed in the enamel surface seemed to have no influence to the bond strengths among self-etch adhesives. Moreover, the thickness of ABRZ appeared to be associated with the amount of fluoride ion released from the primer.

SUMMARY In this laboratory study, the microtensile bond strengths (μTBS) of resin-modified glass ionomer cement (RM-GIC) to sound and artificial caries–affected bovine root dentin (ACAD) using three different conditioning agents were evaluated after 24 hours and three months. The fractured interface was examined with a scanning electron microscope (SEM). Specimens were created on bovine root dentin that was embedded in epoxy resin. For the ACAD specimens, artificial carious lesions were created. The RM-GIC (Fuji II LC) was applied either directly (no treatment), after application of self conditioner, cavity conditioner, or 17% ethylenediamine tetraacetic acid (EDTA) applied for 60 seconds, on sound dentin and ACAD, then light cured. They were stored in artificial saliva for 24 hours or three months. Following this, the specimens were cut into sticks for the μTBS test, and the failure mode of the debonded specimens was examined by using SEM. Pretest failures were excluded from the statistical analysis of the μTBS values because of their high incidence in some groups. Results showed that the μTBS values were significantly affected by the dentin substrate as well as the conditioning agent. Self conditioner provided the highest and most stable μTBS values, while cavity conditioner showed stable μTBS values on sound dentin. Both self conditioner and cavity conditioner had significantly higher μTBS values than the no treatment groups. EDTA conditioning reduced the μTBS after three months to sound dentin, while it showed 100% pretest failure with ACAD for both storage periods.

Modern adhesive systems have been developed for enhanced mechanical and antibacterial properties; however, no such systems contain a calcium source to enhance bond strength. Therefore, we evaluated the effect of an experimental calcium-containing primer (10 wt% CaCl2) in two-step self-etching adhesive systems on micro-tensile bond strength (μ-TBS) and acid resistance in dentin adhesive interface observations after acid-challenge using scanning electron microscopy. Using two types of primers and bonding agents (Clearfil SE Bond primer (SEP), experimental calcium-containing primer (CaP), Clearfil SE Bond (SEB), and Clearfil Protect Bond), we prepared four experimental groups. The μ-TBS of CaP-SEB did not differ from that of SEP-SEB. Meanwhile, the CaP groups showed a thicker acid-base resistance zone. Thus, two-step self-etching adhesive system composed of experimental calciumcontaining primer can be used as an adhesive system with high acid resistance and acceptable bond strength.

This study evaluated the effect of two hemostatic agents on bond strength of resin-modified glass ionomer cement (RMGIC) to root dentin after using different pretreatment solutions compared to resin composite with a 2-step self-etch adhesive. Dentin specimens were either uncontaminated or contaminated with a ferric sulphate or aluminum chloride astringent, RMGIC was applied after conditioning with; Cavity Conditioner, Self Conditioner or Clearfil SE Primer, while a resin composite was bonded using Clearfil SE Bond. Microtensile bond strength (μTBS) values and failure modes were determined. Two-way ANOVA revealed that hemostatic agents did not significantly affect the RMGIC bond strength with any conditioning material (p>0.05). SE Primer pretreatment provided the highest μTBS values among RMGIC groups. For the resin composite, ferric sulphate astringent significantly reduced μTBS value (p≤0.001). Scanning electron micrographs of representative dentin surfaces contaminated with the hemostatic agents showed effects on smear layer removal and dentinal tubule occlusion.

Background: Enamel mineral density is dependent on a balanced dynamic process of demineralization and remineralization. Objective: We evaluated the remineralization potential of experimental calcium- containing primer (CaP) application on enamel subsurface lesions. Methods: Demineralized enamel samples obtained from bovine incisor teeth were prepared and cut buccolingually. All samples were divided into 4 main groups according to the type of primer: CLEARFIL SE BOND 2 Primer (SEP), experimental calcium-containing primer (CaP) and bond: CLEARFIL SE BOND 2 Bond (SEB), CLEARFIL Protect Bond (PBB) treatment: (1) SEP-SEB (2) SEP-PBB (3) CaP-SEB (4) CaP-PBB. Each group was subdivided according to storage time in artificial saliva: immediately, 1 month and 6 months. Then, the samples were analyzed using transverse micro radiography (TMR). Additionally, the samples treated with each primer were prepared for scanning electron microscope (SEM) and energy dispersive X-ray spectroscopy (EDS) observation. Two-way ANOVA was used for the statistical analysis of mineral loss (&Delta, Z: vol%&middot, &micro, m). Results: CaP-PBB had the significantly lowest &Delta, Z at all storage times, while SEP-SEB had the highest &Delta, Z (p &lt, 0.05). SEM observations revealed that new crystals were formed on the surface after 6 months, and the ratio of calcium on the enamel increased in the EDS analysis. Conclusion: Experimental calcium-containing primer can provide additional mineral deposition, with even further deposition when combined with a fluoride-containing bond.

The purpose of this study was to evaluate the early tensile bond strengths of three different resin cements; Super Bond C&B (conventional and quick type) and ResiCem to a CAD/CAM composite block. A CAD/CAM composite block (Shofu Block HC) was ground and silanized according to the manufacturers' instructions before cementation. A conventional tensile bond strength test (O: 4 mm) was performed 10 min, 1 h and 24 h after bonding. Super Bond C&B (quick type) showed the highest bond strength at 24 h. However, results of a three-point bend test showed the mechanical properties were weaker for the Super Bond C&B cements compared with composite cement, Resicem. The 4-META/MMA-TBB resin is a suitable resin cement to bond to a CAD/CAM composite block.

FCP-COMPLEX is a newly developed solution containing fluoride, calcium, and phosphoric acid that has the potential to reinforce caries-affected dentin. This study evaluated the effect of FCP-COMPLEX on micro-tensile bond strength (µTBS) and acid-challenge at the dentin-adhesive interface. FCP-COMPLEX, 2% NaF, and distilled water were applied to artificial caries-affected dentin (ACAD) and the effect on acid-induced damage after resin composite restoration was observed. Scanning electron microscopy and X-ray absorption fine structure (XAFS) were used to evaluate tooth morphology. The µTBS test revealed no effect of FCP-COMPLEX either immediately or after 3 months' storage. The area of acid damage in caries-affected dentin was reduced by FCP-COMPLEX. XAFS analysis revealed that absorbed fluorine on the surface would form CaF2. In conclusion, FCP-COMPLEX significantly reduced the damage of acidic attack at the ACAD-adhesive interface, while the µTBS value was maintained after storage.

Enamel wear, which is inevitable due to the process of mastication, is a process in which the microcracking of enamel occurs due to the surface contacting very small hard particles. When these particles slide on enamel, a combined process of microcutting and microcracking in the surface and subsurface of the enamel takes place. The aim of this study was to detect microscopic differences in the microcrack behavior by subjecting enamel specimens derived from different age groups (immature open-apex premolars, mature closed-apex premolars, and deciduous molars) to cycles of simulated impact and sliding wear testing under controlled conditions. Our findings indicated that the characteristics of the microcracks, including the length, depth, count, orientation, and relation to microstructures differed among the study groups. The differences between the surface and subsurface microcrack characteristics were most notable in the enamel of deciduous molars followed by immature premolars and mature premolars whereby deciduous enamel suffered numerous, extensive, and branched microcracks. Within the limitations of this study, it was concluded that enamel surface and subsurface microcracks characteristics are dependent on the posteruptive age with deciduous enamel being the least resistant to wear based on the microcrack behavior as compared to permanent enamel.

A resin coating technique has been widely advocated in recent years. A combination of a dentin bonding system and a flowable composite is applied on the exposed dentin surfaces immediately after tooth preparation and before taking the final impression. The resin coating is beneficial to both minimize pulpal irritation and enhance the bond strength of a resin cement to dentin. Recently introduced thin-film coating materials based on all-in-one adhesive technology are used for resin coating of crown restorations. Thin-film coating materials can be applied in a single clinical procedure and followed by created a barrier-like film layer on the prepared dentin. Therefore, the resin coating technique may play an important role to protect the dentin phys- ically, chemically, and biologically. The coating materials also have the potential to cover exposed sound enamel and dentin, leading to maximum tooth structure preservation.

This study aimed to investigate an artificial caries-affected dentin (ACAD) model for in vitro bonding studies in comparison to natural caries-affected dentin (NCAD) of human teeth. ACAD was created over 7 days in a demineralizing solution. Mineral density (MD) at different depth levels (0-150 µm) was compared between NCAD and ACAD by transverse microradiography. Micro-tensile bond strengths (µTBS) of two two-step self-etch adhesives to sound dentin, NCAD and ACAD were evaluated. Caries-affected dentin type was not a significant factor when comparing MD at different lesion levels (p>0.05). Under SEM, the dentinal tubules appeared occluded with crystal logs 1-2 µm in thickness in the NCAD; whereas they remained open in the ACAD. The µTBS to caries-affected dentin was lower than sound dentin, but was not affected by the type of caries (p>0.05). In spite of their different morphologies, the ACAD model showed similar MD and µTBS compared to NCAD.

This study aimed to investigate the effect of fluoride concentration in adhesives on morphology of acid-base resistant zone (ABRZ). Seven experimental adhesives with different concentrations of NaF (0 wt%; F0 to 100 wt%: F100) were prepared based on the formulation of a commercially available adhesive (Clearfil Protect Bond, F100). The resin-dentin interface of the bonded specimen was subjected to demineralizing solution and NaOCl, sectioned, polished and argon-ion etched for SEM observation. Fluoride release from each adhesive was measured using an ion-selective electrode. Fluoride ion release from the adhesive linearly increased with higher NaF concentration. The ABRZ area increased significantly with higher NaF concentration except for F0, F10, and F20 (p

Although the demand for aesthetic restoration of primary molars has increased, the full-crown restorations using resin and the details of the wear characteristics of trimethylolpropane trimethacrylate (TMPT) filler containing resins for primary molars are not well understood. This study was conducted to determine whether new light-cured composite resin (Fantasista) and 4-META/MMATBB resin (Bondfill SB) are appropriate for full crown restoration of primary molars by evaluating their wear characteristics. Both resins products contain TMPT filler. The properties of the resins were evaluated through in vitro impacting-sliding wear tests; the wear properties of the opposing enamel specimens used in the tests were also studied. The properties of the resins were compared with those of Litefill, MetafilC, and Clearfil FII, which had been evaluated previously. Fantasista exhibited simple shape of wear that was suggestive of a higher wear resistance than that of Litefill. Fantasista caused the least damage to the antagonistic primary enamel.

The purpose of this study was to evaluate bonding performance and dentin interface acid resistance using a 4-META/MMA-TBB based restorative material (BF) compared to a conventional 4-META/MMA-TBB resin cement (SB), and the effect of sodium fluoride (NaF) addition to the materials. Dentin surfaces were treated with 10% citric acid-3% ferric chloride (10-3) or 4-META containing self-etching primer (TP), followed by application of BF or SB polymer powders with or without NaF, to evaluate microtensile bond strength (µTBS) in six experimental groups; 10-3/SB, 10-3/BF, TP/SB, TP/BF, TP/SB/NaF and TP/BF/NaF. SEM observation of the resin-dentin interface was performed after acid-base challenge to evaluate interfacial dentin resistance to acid attack. TP/BF showed highest µTBS, while NaF polymers decreased µTBS. TP/BF showed funnel-shaped erosion at the interface, however, NaF polymers improved acid resistance of interface. In conclusion, BF demonstrated high µTBSs and low acid-resistance at the interface. NaF addition enhanced acid resistance but decreased µTBS.

This study investigated the influence of the composition of self-etching primer adhesive systems on the morphology of acid-base resistant zones (ABRZs). One-step self-etching primer systems (Clearfil Tri-S Bond, G-Bond, and One-Up Bond F Plus) and two-step self-etching primer systems (Clearfil SE Bond, Clearfil Protect Bond, UniFil Bond, and Mac Bond II) were used in this study. Each adhesive was applied on prepared dentin disk surfaces, and a resin composite was placed between two dentin disks. All resin-bonded specimens were subjected to acid-base challenge. Observation under a scanning electron microscope (SEM) revealed the creation of an ABRZ adjacent to the hybrid layer for all the self-etch primer adhesive systems, even when non-fluoride releasing adhesives were used. The presence of fluoride in two-step self-etching adhesive significantly increased the thickness of ABRZ created. Results suggested that an ABRZ was created with the use of self-etching primer adhesive systems, but its morphology differed between one-and two-step self-etching primer adhesive systems and was influenced by fluoride release activity.

Summary Dentin bonding systems have been dramatically simplified and improved during the recent decades. Monomer penetration into dentin and its polymerization in situ creates a hybrid layer, which is essential to obtain good bonding to dentin. Moreover, the presence of an acid–base resistant zone below the hybrid layer has been documented with self-etching adhesive systems in an artificial secondary caries attack. When ultrastructure of the acid–base resistant zone is assessed by SEM and TEM observations, formation of the acid–base resistant zone is considered to be due to the monomer penetration potential and fluoride release in the adhesive systems. Natural dentin has a limited potential to resist an acid attack of secondary caries; however, the acid–base resistant zone does not purely consist of dentin in morphology, it is rather a combination of dentin and the adjacent hybrid layer. Therefore, the reinforced dentin has been called "Super Dentin" bearing the ability to prevent primary and secondary caries. Prospectively, the great potential of adhesive technology in creation of the "Super Dentin" would lead to the development of new materials for mechanical, chemical and biological protection of the dental structures.

This study examined the ultrastructure of both intact and caries affected dentin-adhesive interface after artificial secondary caries formation, using scanning electron microscopy and nanoindentation testing. Half of the prepared specimens were bonded with Clearfil SE Bond (Kuraray Medical, Japan) and a resin composite (Metafil Flo, Sun Medical, Japan) for the nanoindentation test. The other specimens were stored in a buffered demineralizing solution for 90 minutes, then observed using SEM. An acid-base resistant zone (ABRZ) was observed beneath the hybrid layer, distinguished by argon-ion etching. The ABRZ of caries-affected dentin was thicker than that of normal dentin, while its nanohardess was lower than normal dentin (p0.05). It is suggested that the monomer of Clearfil SE Bond penetrated deeper than previously reported, creating a so-called "hybrid layer." However, its physical properties depended on the condition of the dentin.

This study evaluated the influence of a fluoride-containing adhesive on microtensile bond strength (microTBS) to dentin, as well as analyzed the dentin-adhesive interface after acid-base challenge. Experimental groups were: G1--Clearfil SE Bond control (SE); G2--Clearfil Protect Bond control (PB); G3--Primer[SE]/Adhesive[PB]; G4--Primer[PB]/Adhesive[SE]. For microTBS evaluation, dentin surfaces were ground, bonded, and composite resin crowns were built up to obtain beams to be tested. For interfacial analysis, adhesive system was applied on dentin surface and a low-viscosity resin was placed between two dentin disks. Then, the specimens were subjected to acid-base challenge, sectioned, and polished to be observed by SEM. microTBS data showed no statistical differences among the groups (GI: 51.3, G2: 47.6, G3: 55.0, G4: 53.9; mean in MPa). Through SEM, it was observed that a thick acid-base resistant zone adjacent to the hybrid layer was created only when the fluoride-releasing adhesive was used. In conclusion, the presence of fluoride in an adhesive contributed significantly to preventing secondary caries, and did not interfere with dentin-adhesive bond strength.

The purpose of this study was to investigate the mechanical properties of intertubular dentin in sound, natural caries-affected (NCAD) and artificial caries-affected dentin (ACAD) using nanoindentation.Non-caries molars and caries molars with International Caries Detection and Assessment System (ICDAS II) score 5 at the occlusal site were used and caries was excavated using a spoon excavator, a round bur at low speed without water and a dye solution as guidance to detect the infected tissue. Specimens with remaining dentin thickness (RDT)2mm were selected. ACAD teeth were created from sound teeth over 7 days in a demineralizing solution. Specimens were embedded into plastic rings with acrylic resin and then sagittal mesial-distal sectioned from crown to the long axis of the root under cooling water using a low-speed diamond blade. The surface of interest was fine polished sequentially. Hardness measurement was performed within an axial depth of 1000μm with at least of 320 indentations on each sample. Mann-Whitney U Test was used to compare the hardness as the variable among different dentin types (SOUND, NCAD and ACAD) at each dentin depth level.There was no significant difference in nanohardness between NCAD and ACAD up to a depth of 130μm (p0.05). NCAD consistently showed lower hardness. ACAD showed no significant difference in hardness with SOUND dentin beyond 190μm (p0.05). The lesion front in ACAD was considered to be located around the depth of 180μm.Natural and artificial caries-affected dentin tissues were superficially comparable in intertubular nanohardness. There is a certain layer within the natural caries-affected dentin with higher hardness; however the long-term effects of caries beneath the lesion extend deeply through intertubular dentin. Sound dentin at deep areas (close to the pulp chamber) is considered to be soft.

An acid-base resistant zone has been found to exist after acid-base challenge adjacent to the hybrid layer using SEM. The aim of this study was to examine the acid-base resistant zone using three different bonding systems. Dentin disks were applied with three different bonding systems, and then a resin composite was light-cured to make dentin disk sandwiches. After acid-base challenge, the polished surfaces were observed using SEM. For both one- and two-step self-etching primer systems, an acid-base resistant zone was clearly observed adjacent to the hybrid layer - but with differing appearances. For the wet bonding system, the presence of an acid-base resistant zone was unclear. This was because the self-etching primer systems etched the dentin surface mildly, such that the remaining mineral phase of dentin and the bonding agent yielded clear acid-base resistant zones. In conclusion, the acid-base resistant zone was clearly observed when self-etching primer systems were used, but not so for the wet bonding system.

The aim of this study was to evaluate the effects of coating root dentin surfaces with adhesives vis-a-vis the prevention of root dentin demineralization. Root dentin surface was ground with #600 SiC, and then either a single coat of Clearfil SE Bond (SE), Clearfil Tri-S Bond (TS), G-Bond (GB), Hybrid Bond (HB-1), or two coats of HB (HB-2) were applied. Specimens were immersed in an artificial demineralizing solution, then sectioned through the center of the root and polished. Thickness of the coating layer and depth of the demineralized dentin layer were observed under a confocal laser scanning microscope (CLSM). Nanohardness values of the coating layer and underlying dentin were measured using a nanoindentation tester. All obtained data were statistically analyzed. Dentin demineralization was not observed in the surface coating groups with the exception of HB-1, and nanohardness of the underlying dentin was comparable to that of normal dentin. Based on the results obtained, it seemed that coating root dentin surfaces with an adhesive material is a promising good practice to prevent demineralization.

An acid-base resistant zone (ABRZ) has been shown to be created under a hybrid layer in a self-etching adhesive system at the adhesive/dentin interface. The purpose of this study was to assess the nanostructure of the ABRZ by applying all-in-one adhesive systems. Human premolar dentin was treated with one of two all-in-one adhesive systems; Clearfil Tri-S Bond and G-Bond according to the manufacturers' instructions. After placement of a resin composite, the bonded interface was vertically sectioned and subjected to an acid-base challenge. Following this, the nanostructure of the ABRZ was examined by SEM and TEM. The SEM observations of the adhesive-dentin interface after the acid-base challenge indicated that a hybrid layer less than 1 mum thick was created, and a ABRZ was formed beneath the hybrid layer for each adhesive system. The TEM observations indicated that the ABRZ contained mineral components in both adhesive systems, however, the thickness of the ABRZ was material dependent. The application of the all-in-one adhesive systems created an ABRZ at the underlying dentin, which reinforced normal dentin against dental caries. Therefore, this zone was named 'Super Dentin'. Formation of 'Super Dentin' is a new approach in caries prevention.

The purpose of this study was to evaluate dentin bond strengths and to observe the adhesive-dentin interface after acid-base challenge using fluoride-free and fluoride-releasing self-etching adhesive systems; Clearfil SE Bond (SE), FL-Bond (FL) and FL-Bond II(FL II). Fifteen dentin surfaces from human molars were ground and bonded with one of three adhesive systems. The microtensile bond strength (muTBS) test was performed at a crosshead speed of 1 mm/min. The interface of the bonded specimens after acid-base challenge were also examined by a SEM. The muTBS of SE were significantly higher than those of FL and FL II (p0.05), however, there were no significant differences between FL and FL II (p0.05). An acid-base resistant zone (ABRZ) was observed in all the groups, however, formation of the ABRZ was material dependent. Fluoride-release from the adhesive is a key factor to create thick ABRZ.