Micromorphological changes in resin-dentin bonds after 1 year of water storage

The purpose of this study was to evaluate the degradation of resin-dentin bonds after 1 year of water storage. Resin-dentin-bonded specimens were prepared with the use of an adhesive resin system (One-Step: Bisco). Half of the experimental specimens were sectioned perpendicular to the adhesive interface to produce a beam (adhesive area: 0.9 mm(2)) before being stored in distilled water at 37 degrees C for 1 year. The remaining half of the bonded specimens were sectioned into beams of similar dimensions after 1 year of water storage. Additional bonded specimens that had been stored in water for 24 h before sectioning into beams were used as controls. The beams in the two experimental groups and the control group were subjected to microtensile bond testing. Fractography was performed on all fractured beams with the use of FE-SEM. There were significant (p <.05) differences in bond strength among the control specimens (55.9 +/- 12.9 MPa), specimens that had been sectioned into beams after water storage (68.9 +/- 18.6 MPa), and specimens that had been sectioned into beams before water storage (28.1 +/- 9.3 MPa). Fractography revealed that the resin material was gradually extracted from the periphery to the center portion of the beam. This probably accounted for the decrease in bond strength after 1 year of water storage.     

Deproteinizing effects on resin-tooth bond structures

This study investigated the effects of NaOCl on resin-tooth bonds to simulate the situations of long-term durability and caries invasion. Resin-tooth bonded specimens were produced with the use of two resin adhesives (Excite and One-Bond). Resin-tooth bonded beams (adhesive area; 0.9 mm2) were serially sectioned and the specimens were immersed in 10% NaOCl medium for 0 (control), 2, 4, and 6 h after being stored in water for 24 h. After immersion, microtensile bond tests were performed. SEM fractography was conducted to calculate each failure mode by image analysis. In addition, the adhesive interface was examined with the use of TEM. In the control specimens, enamel bond strengths had no difference between Excite (45.6 +/- 15.0) and One-Bond (56.9 +/- 12.9). On the other hand, dentin bond strengths had significant difference between Excite (80.6 +/- 21.2) and One-Bond (50.7 +/- 11.2). The bond strengths decreased with increased storage time for both systems with enamel and dentin bonds. The deteriorated mineralized dentin of beams resulted in bond-strength reduction for resin-enamel bonds. For dentin bonding, the adhesive interface was gradually dissolved from the outer to the center portion of the beam. The depletion of collagen fibrils within the demineralized dentin or hybrid layer deformation was found under SEM and TEM examinations. These morphological changes are responsible for bond strength reduction of resin-dentin bonds.     

SEM and TEM analysis of water degradation of human dentinal collagen

Recently several long-term studies have reported evidence of the hydrolytic degradation of collagen fibrils based on fractured surface observations after bond testing. Those studies suggested that one cause of the decline in the bond strength was the degradation of the collagen fibrils within the bonds. However, one concern has been raised that the dentinal collagen fibrils may be stable in water that does not contain oral bacteria or enzymes. Therefore, the present study aimed to clarify the micromorphological change in naked collagen fibrils after 500 days of water storage. To prepare exposed collagen fibrils, sectioned and polished human dentin surfaces were acid conditioned for 15 s with the use of two commercially available acid conditioners: All-Etch (10% phosphoric acid) and Uni-Etch (32% phosphoric acid) (Bisco, Inc.). Those specimens were stored in distilled water at 37 degrees C for 1 day (control) for 500 days. After the storage periods, the samples were examined with the use of SEM and TEM. Under SEM and TEM examination, micromorphological alterations (disarrangement of collagen web, widening the interfibrillar space, and the thinning diameter of collagen fibrils) were found in the specimens after 500 days in water.     

In vitro effect of nanoleakage expression on resin-dentin bond strengths analyzed by microtensile bond test, SEM/EDX and TEM

This study evaluated the effect of multiple consecutive adhesive resin coatings of adhesive bonded to human dentin on nanoleakage and resin-dentin bond strength. Resin bonded dentin specimens were prepared using a total-etch adhesive (One-Step Plus) applied as multiple consecutive coating, or using two self-etch adhesive systems (iBond or Fluoro Bond). For the total-etch adhesive, resin application and air evaporation were performed 1, 2, 3, or 4 times. The self-etch adhesives were applied according to manufacturers' instructions. Resin-dentin bonded beams were prepared and immersed in water (control) or ammoniacal silver nitrate. After storage, microtensile bond strengths were measured. The fractured surfaces were examined by scanning and transmission electron microscopy (SEM and TEM), and energy-dispersive X-ray spectrometry (EDX). No significant differences in bond strength were found between water and silver nitrate storage groups. Several types of silver depositions (spotted, reticular, or water trees) were found in adhesive joints. The bond strengths of the single coated specimens of the total-etch adhesive were significantly lower than those receiving 2-4 coatings. Single coats produced more nanoleakage than multiple coats. However, no correlation was found between the bond strengths and nanoleakage between the different adhesives (total-etch adhesive with different conditions or self-etch adhesives).     

Biomimetic remineralization as a progressive dehydration mechanism of collagen matrices – Implications in the aging of resin–dentin bonds

Biomineralization is a dehydration process in which water from the intrafibrillar compartments of collagen fibrils are progressively replaced by apatites. As water is an important element that induces a lack of durability of resin–dentin bonds, this study has examined the use of a biomimetic remineralization strategy as a progressive dehydration mechanism to preserve joint integrity and maintain adhesive strength after ageing. Human dentin surfaces were bonded with dentin adhesives, restored with resin composites and sectioned into sticks containing the adhesive joint. Experimental specimens were aged in a biomimetic analog-containing remineralizing medium and control specimens in simulated body fluid for up to 12 months. Specimens retrieved after the designated periods were examined by transmission electron microscopy for the presence of water-rich regions using a silver tracer and for collagen degradation within the adhesive joints. Tensile testing was performed to determine the potential loss of bond integrity after ageing. Control specimens exhibited severe collagen degradation within the adhesive joint after ageing. Remineralized specimens exhibited progressive dehydration, as manifested by silver tracer reduction and partial remineralization of water-filled microchannels within the adhesive joint, as well as intrafibrillar remineralization of collagen fibrils that were demineralized initially as part of the bonding procedure. Biomimetic remineralization as a progressive dehydration mechanism of water-rich, resin-sparse collagen matrices enables these adhesive joints to resist degradation over a 12-month ageing period, as verified by the conservation of their tensile bond strength. The ability of the proof of concept biomimetic remineralization strategy to prevent bond degradation warrants further development of clinically relevant delivery systems.     

Diffusion-induced water movement within resin-dentin bonds during bonding

It is thought that water-filled channels and nanovoids in resin-dentin bonds represent potential sites for degradation of bonds or hydrolysis of collagen or both. How water gains access to bonded interfaces is not clear. This study evaluated the diffusion-induced water uptake through resin-dentin interfaces during bonding. Two light-cured total-etch adhesive systems (Excite and One-Step Plus) and a chemical-cured adhesive (Amalgambond Plus) were used in this study. Dentin disks were placed in a split-chamber device, and the fluid movement across dentin was measured, with and without a physiological pressure, during bonding procedures and 24 h after bonding. For light-cured adhesives in the experimental groups, a 6 min interval of dark storage was conducted prior to light-curing, to evaluate the diffusion of water through the uncured resin monomers, and to test the effect of prolonged infiltration time of adhesives on water permeability of bonds. Prolonged adhesive infiltration reduced the water permeability of resin-dentin bonds for light-cured adhesives. Water gradients produced by bonding systems contribute to water movement across the dentin-adhesive interfaces during bonding procedures. Differences in chemical formulations for adhesive systems may lead to differences in the extent of diffusion-induced water movement and the amount of water within the resin-dentin bonds.     

The importance of size-exclusion characteristics of type I collagen in bonding to dentin matrices

The mineral phase of dentin is located primarily within collagen fibrils. During development, bone or dentin collagen fibrils are formed first and then water within the fibril is replaced with apatite crystallites. Mineralized collagen contains very little water. During dentin bonding, acid-etching of mineralized dentin solubilizes the mineral crystallites and replaces them with water. During the infiltration phase of dentin bonding, adhesive comonomers are supposed to replace all of the collagen water with adhesive monomers that are then polymerized into copolymers. The authors of a recently published review suggested that dental monomers were too large to enter and displace water from collagen fibrils. If that were true, the endogenous proteases bound to dentin collagen could be responsible for unimpeded collagen degradation that is responsible for the poor durability of resin–dentin bonds. The current work studied the size–exclusion characteristics of dentin collagen, using a gel-filtration-like column chromatography technique, using dentin powder instead of Sephadex. The elution volumes of test molecules, including adhesive monomers, revealed that adhesive monomers smaller than ～1000 Da can freely diffuse into collagen water, while molecules of 10,000 Da begin to be excluded, and bovine serum albumin (66,000 Da) was fully excluded. These results validate the concept that dental monomers can permeate between collagen molecules during infiltration by etch-and-rinse adhesives in water-saturated matrices.     

Differential effect of in vitro degradation on resin-dentin bonds produced by self-etch versus total-etch adhesives

OBJECTIVE: To evaluate the effect of an in vitro challenge (NaOCl immersion) on microtensile bond strength (MTBS) of five adhesive systems to dentin. METHODS: Flat dentin surfaces from 40 molars were bonded with three total-etch adhesives (Single Bond, Prime&Bond NT and the experimental Prime&Bond XP), and two self-etching agents (Clearfil SE Bond and Etch&Prime 3.0). Composite build-ups were constructed with Tetric Ceram. Teeth were then sectioned into beams of 1.0 mm2 cross-sectional area. Half of the beams were immersed in 10% NaOCl aqueous solution for 5 h. Each beam was tested in tension in an Instron machine at 0.5 mm/min. Data were analyzed by 2-way ANOVA and multiple comparisons tests (p < 0.05). RESULTS: Clearfil SE Bond and Single Bond attained higher MTBS than the other three adhesives. Prime&Bond NT and Prime&Bond XP performed equally, and Etch&Prime resulted in the lowest MTBS. After NaOCl immersion, MTBS decreased in all groups. The highest MTBS values were obtained for Clearfil SE Bond and Prime&Bond XP. Scaning electron microscopy observation of debonded sticks evidenced dissolution and microstructural alterations of intertubular dentin, except when Clearfil SE Bond was used. CONCLUSIONS: Resin-dentin bonds are prone to chemical degradation. The extent of the resin degradation is adhesive system specific. Chemical degradation of the nonresin infiltrated collagen fibers does also exist in total-etch adhesives. Both processes may reduce long-term resin-dentin bond strength.     

Degradation patterns of different adhesives and bonding procedures

Various types of resin adhesives and procedures are available in the clinical field, so comprehensive understanding of degradation is required for each material and bonding procedure. The objective of this study was to investigate the bond durability for different adhesives and bonding procedures. Resin-dentin bonded beams were prepared with the use of two adhesives (One-Up Bond F/self-etching primer system and One Bond/total-etch adhesive) and two experimental groups for the bonding procedure (wet and dry bonding of the total-etch adhesive). Those samples were soaked in water for 24 h(control), 6 and 12 months. After the water immersion, the bond strengths were measured by the microtensile bond test, and subsequently fractography was performed with the use of SEM. Statistically significant reduction of the bond strength (p < 0.05) was apparent after 12 months of water exposure in the range 22-48% of the control. The bonding resin was eluted from the hybrid layer of the self-etching and the total-etch adhesives for the wet bonding. Micromorphological alterations were found due to the hydrolysis of collagen fibrils with the total-etch adhesive for the dry bonding mode. These pathologic alterations were in accord with the bond strength.     

Bonding characteristics of newly developed all-in-one adhesives

This study evaluated the microtensile bond strength and the interfacial morphology of newer adhesives. The occlusal surfaces of extracted teeth were ground flat for random allocation to four equal groups. Resin composite was bonded to each surface using either Clearfil SE Bond [SEB], Clearfil Protect Bond [PB], G-Bond [GB], or an experimental adhesive, SSB-200 [SSB]. After storage for 24 h in water at 37 degrees C, they were sectioned into beams (cross-sectional area 1 mm(2)) for microtensile bond strength testing (muTBS) at a crosshead speed of 1 mm/min. The load at failure of each was recorded; the data were analyzed by one-way ANOVA and Games Howell tests. The surfaces of the fractured specimens were observed using SEM. For the ultra-morphology of the interface, the occlusal surfaces of four more teeth were prepared as before and a thin layer of flowable resin composite was bonded to each surface using one of the four adhesives.The mean muTBS ranged from 39.68 MPa (GB) to 64.97 MPa (SEB). There were no statistical differences between SEB and SSB, or between PB and GB (p > 0.05). The muTBS of SEB and SSB were significantly greater than that of PB and GB (p < 0.05). SEMs of the fractured surfaces revealed a mixed (cohesive/interfacial) failure. TEM examination highlighted differences in the hybrid layer; SEB had a thicker layer than the others. In conclusion, the newer all-in-one adhesives produced a thin hybrid layer but varied in their bond strengths. The 2-step self-etching adhesives do not necessarily produce higher bond strengths than that of the all-in-one systems.     

Effects of a peripheral enamel bond on the long-term effectiveness of dentin bonding agents exposed to water in vitro

This study evaluated the effects of water exposure on the in vitro microtensile bond strength (muTBS) of etch-and-rinse and self-etching adhesives to human dentin over a 1-year storage period. Five adhesive systems used were as follows: a one-step self-etching adhesive (One-up Bond F-OB), two two-step self-etching primers (Clearfil SE Bond-SE and Clearfil Protect Bond-CP), and two etch-and-rinse adhesives (Single Bond-SB and Prime&Bond NT-PB). Dentin surfaces were bonded, restored, and assigned to four subgroups, according to the degree of water exposure: 24 h of peripheral water exposure (24 h-PE) (having circumferential enamel); and 1 year of peripheral exposure (1 yr-PE), direct exposure (1 yr-DE) (dentin directly water-exposed), or directly exposed to oil only (no water exposure) (1 yr-DOE). A composite-enamel bond adjacent to the restoration is determined if the water exposure was peripheral or direct. After storage periods, specimens were serially sectioned, trimmed to an hourglass shape with a cross-sectional area of 1 mm(2) at the interface, and tested in tension. Results were analyzed by two-way ANOVA and Tukey test (alpha = 0.05). No difference was found between 24 h-PE and 1 yr-PE for OB, CP, SB, and PB. However, muTBS values significantly dropped after 1 yr-DE for SE, CP, SB, and PB. A decreased muTBS was seen in SE after 1 yr-PE, but no differences existed between 1 yr-PE and 1 yr-DE. Similar or increased muTBS values were noted in 1 yr-DOE for all adhesives. Water-storage for 1 year significantly decreased muTBS for all adhesives. However, except for SE, the presence of a peripheral composite-enamel bond seemed to reduce the degradation rate in resin-dentin interfaces for all materials.     

Effect of structural change of collagen fibrils on the durability of dentin bonding

This study investigates the effect of structural changes of collagen fibrils on the bonding durability of a total etch luting resin (Super-Bond C&B) and a self-etching luting resin (Panavia F 2.0) to dentin. An atomic force microscope (AFM) was used to observe structural changes of intact dentin collagen fibrils after acidic conditionings of two bonding systems. After 90 d water storage and 15,000 thermal cycles (TC) as artificial aging, micro-tensile bond strength (microTBS) was utilized to evaluate the bonding durability of the two bonding systems to dentin. microTBS after 1 d or 90 d water storage without TC were separately measured in control groups. A cross-banding periodicity of about 67 nm along collagen fibrils was seen on demineralized intertubular dentin surfaces in AFM images. For both luting resins, thermal cycling decreased (p < 0.05) microTBS of 1 d and 90 d, compared to controls. Scanning electron microscope and transmission electron microscopic examinations revealed that the top and bottom of hybrid layer (HL) were weak links in the bonding interface over time. The results suggest that the top of HL contains disorganized collagen fibrils from the smear layer which degrade over time. AFM results indicate that the demineralized intact collagen fibrils beneath the smear layer were not denatured during acidic conditioning. However, these collagen fibrils may be structurally unstable due to poor infiltration by resin or loss of resin protection within the HL over time, reducing the long-term microTBS. This process was accelerated by thermal fatigue cycling.     

Elemental distributions and microtensile bond strength of the adhesive interface to normal and caries-affected dentin

The aim of this study was to evaluate the microtensile bond strength (microTBS) and the elemental contents of the adhesive interface created to normal versus caries-affected dentin. Extracted human molars with coronal carious lesions were used in this study. A self-etching primer/adhesive system (Clearfil Protect Bond) was applied to flat dentin surfaces with normal and caries-affected dentin according to the manufacturer's instructions. After 24 h water storage, the bonded specimens were cross-sectioned and subjected to a microTBS test and electron probe microanalysis for the elemental distributions [calcium (Ca), phosphorus (P), magnesium (Mg), and nitrogen (N)] of the resin-dentin interface after gold sputter-coating. The microTBS to caries-affected dentin was lower than that of normal dentin. The demineralized zone of the caries-affected dentin-resin interface was thicker than that of normal dentin (approximately 3 microm thick in normal dentin; 8 microm thick in caries-affected dentin), and Ca and P in both types of dentin gradually increased from the interface to the underlying dentin. The caries-affected dentin had lost most of its Mg content. The distributions of the minerals, Ca, P, and Mg, at the adhesive interface to caries-affected dentin were different from normal dentin. Moreover, a N peak, which was considered to be the collagen-rich zone resulting from incomplete resin infiltration of exposed collagen, was observed to be thicker within the demineralized zone of caries-affected dentin compared with normal dentin.     

Degradation of the resin-dentin bonds after simulated and inhibited cariogenic challenge in an in situ model

The aim of this study was to evaluate the resin-dentin bonds of two simplified etch-and-rinse adhesive after simulated cariogenic and inhibited cariogenic challenge in situ. Dental cavities (4 mm wide, 4 mm long, and 1.5 mm deep) were prepared in 60 bovine teeth with enamel margins. Restorations were bonded with either adhesive Adper Single Bond 2 (3MESPE) or Optibond Solo Plus (Kerr). Forty restorations were included in an intra-oral palatal appliance that was used for 10 adult volunteers while the remaining 20 dental blocks were not submitted to any cariogenic challenge [NC group] and tested immediately. For the simulated cariogenic challenge [C+DA], each volunteer dropped 20% sucrose solution onto all blocks four times a day during 14 days and distilled water twice a day. In the inhibited cariogenic challenge group [C + FA], the same procedure was done, but slurry of fluoride dentifrice (1.100 ppm) was applied instead of water. The restored bovine blocks were sectioned to obtain a slice for cross-sectional Vickers microhardness evaluation and resin-dentin bonded sticks (0.8 mm(2)) for resin-dentin microtensile evaluation. Data were evaluated by two-way ANOVA and Tukey's tests (α = 0.05). Statistically lower microhardness values and degradation of the resin-dentin bonds were only found in the C + DW group for both adhesives. The in situ model seems to be a suitable short-term methodology to investigate the degradation of the resin-dentin bonds under a more realistic condition.     

The bond strength of light-curing composite resin to finally polymerized and aged glass fiber-reinforced composite substrate

OBJECTIVE: This study examines the shear bond strength of visible light-curing composite resin (VCR) to aged glass fiber-reinforced composite (FRC) substrate with multi-phase polymer matrix. METHODS: Linear polymethyl methacrylate and dimethacrylate monomer preimpregnated unidirectional glass fiber reinforcement was used as an adhesion substrate for low-viscosity diacrylate veneering composite resin and restorative composite resin. A total of 60 test specimens were divided into three groups according to the brand and the use of an intermediate monomer resin (IMR). The used IMRs were either BisGMA-HEMA-resin, BisGMA-TEGDMA resin or the controls were left without the IMR treatment. Dry- and water-stored FRC-substrates were used for adhering the VCR with or without the IMR. The shear bond strength of the VCR to the substrate was measured for dry and thermocycled specimens and the results were analyzed with multi-variate ANOVA. RESULTS: The highest mean shear bond strength (23.9 +/- 4.8 MPa) was achieved with FRC/BisGMA-HEMA/VCR combination when the FRC substrate was water stored and the test specimen was thermocycled. FRC/BisGMA-TEGDMA/VCR combination resulted in 15.7 +/- 6.0 MPa with the water-stored FRC substrate and after thermocycling of the test specimens. The lowest shear bond strength (1.0 +/- 0.5 MPa) was obtained with FRC/VCR combination with water-stored substrate and after thermocycling of the test specimens. Significant differences were found between the mean values of three groups according to the use of IMR (p<0.001). The storage conditions of the FRC substrate were related to brand of the IMR or the composite (p<0.001). High mean values of the shear bond strength after thermocycling fatigue were related to the type of IMR (p<0.001). SIGNIFICANCE: The results suggest that the IMRs used in this study greatly influence the mean shear bond strength values when the test specimens are thermocycled.     

Influence of organic acids present in the oral biofilm on the microtensile bond strength of adhesive systems to human dentin

This study evaluated the influence of organic acids present in the oral biofilm on the microtensile bond strength (μTBS) of adhesive systems to human dentin. Sixty occlusal dentin surfaces were wet ground with 600 grit SiC abrasive paper and divided into four groups according to the adhesive systems: Scotchbond Multipurpose (SMP), Adper Single Bond 2, Adper Scotchbond SE (ASE), and Clearfill SE Bond (CSE). After the adhesive systems were applied, a block of resin composite was built up on the dentin surfaces. After 24 h storage in distilled water at 37°C, the teeth were perpendicularly cut to obtain beams (1 mm(2)). For each adhesive system, the beams were divided into three groups according to storage media: artificial saliva (AS); propionic acid (PA), and lactic acid (LA). After 7 days storage at 37°C, the beams were submitted to μTBS testing. The μTBS ranged from 36.0 ± 1.6 (ASE-PA) to 52.5 ± 1.2 (CSE-AS). For all adhesive systems, the μTBS values after storage in PA were lower than those in AS. Except for the SMP, the values of μTBS after storage in LA were lower than those in AS. The adhesive ASE presented the lowest values of μTBs in the three media. The acids present in the oral biofilm may affect the bond strength of adhesive systems to human dentin.     

Effect of load cycling and in vitro degradation on resin-dentin bonds using a self-etching primer

The objective of this study was to evaluate the effect of in vitro degradation and mechanical loading on microtensile bond strength (MTBS) and microleakage (ML) of a resin composite to dentin using a self-etching primer adhesive [Clearfil SE Bond (SEB)] under two hydration statuses. Twenty-four flat dentin surfaces were divided in groups: 1) blot-dried, 2) air-dried. SEB was applied and resin buildups were performed with Tetric Ceram. Specimens were divided in four subgroups: a) sectioned into beams, b) load cycled, c) beams were immersed in NaOCl for 5 h, d) load cycled and immersed in NaOCl. Beams were tested in tension. For ML testing, 80 Class V cavities were prepared and molars divided in subgroups as described above (in group c and d, specimens were kept in distilled water for 1 year, instead of the 5-h NaOCl immersion). ML was assessed by dye penetration. Analysis of variance and multiple comparisons tests were used for MTBS. For ML, Mann-Whitney U and Wilcoxon matched pairs signed ranked were used (p<0.05). SEB applied to completely dehydrated dentin produced the highest MTBS, at 24-h evaluation. In vitro degradation always decreased MTBS, and fatigue loading only diminished MTBS on dehydrated dentin. Load cycling increased dye penetration on dentin margins. Degradation always increased ML in both enamel and dentin margins.     

Micromorphological analysis of the interaction between a one-bottle adhesive and mineralized primary dentine after superficial deproteination

It has been claimed that resin monomers may incompletely penetrate into demineralized collagen network, which could form a weak hybrid layer. In consequence, it has been proposed that removal of the exposed collagen network could improve adhesion to dentine. The interface between a water/ethanol-based one-bottle adhesive (Single Bond, 3M) which is devoid of acid monomers, and deproteinated surface of primary dentine was evaluated by SEM. Dentine disks were obtained from 20 primary teeth. Two disks were used to standardize the application time of sodium hypochlorite (NaOCl) for getting an effective deproteination. The remaining 18 disks were equally divided into two groups and treated as follows: control group (CG) 35% phosphoric acid (PA) for 15s; treated group/deproteination (TG) 35% PA for 15s+10% NaOCl for 3 min. Single Bond and Z250 (3M) were placed on all disks according to the manufacturer's instructions. The 18 resin-dentine disks were fractured to obtain hemi-disks and processed for SEM. The examination of the CG specimens showed a typical hybrid layer and the presence of numerous tags with few and short microtags. The TG specimens, which did not present hybrid layer, also exhibited numerous tags, with few and short microtags. Some areas between the tags showed fibrillar-like projections, which appeared to be mineralized collagen fibrils, which were incorporated into the adhesive. Thus, our results suggest that some chemical interaction may occur between mineralized dentinal collagen and the adhesive used.     

Effect of acidic pretreatment combined with a silane coupling agent on bonding durability to silicon oxide ceramic

This study examined the effect of different acidic treatments and the role of a phosphate monomer in a silane coupling agent on the durability of the dual-cure resin cement/silicon oxide bond. Ceramic blocks (Vita Celay Blanks) were cut into multiple 3 mm-thick slices and polished using 600 grit SiC paper. Two pairs were left untreated [controls (CTRL)], two pairs were treated with 40% phosphoric acid and rinsed with water for 30 s (PA), and another two pairs treated with 20% hydrofluoric acid followed by 30 s water rinsing (HF). Half the specimens were silanated with Tokuso Ceramics Primer (TCP) (Tokuyama) and the other half with TCP formulated without phosphate monomer (TCP-NoPM). All the pairs were bonded with Bistite II dual-cure resin cement (Tokuyama) and light cured. After 24 h water storage at 37 degrees C, 0.7 mm-thick slabs were serially sectioned. Immediately, after 6 months and after 1 year of water storage, two slabs were randomly selected from each subgroup, and sliced into beams (6 x 0.7 x 0.7 mm) for the microtensile bond strength (muTBS) test. The muTBS data were statistically analyzed using multiple Wilcoxon Signed Rank tests (p < 0.05). Failure modes were determined using a confocal laser-scanning microscope. Ceramic surface morphology after the different acidic treatments was examined using an SEM. After 1 day, in the case of silane treatment with TCP, there were no significant differences in muTBS between the control and acid-treated groups (p > 0.05), whereas with TCP-NoPM, the muTBS of the control was significantly lower than the acid-treated groups (p < 0.05). All the TCP and acid-treated TCP-NoPM groups exhibited significant reductions in muTBS after 6 months (p < 0.05). After 1 year, the muTBS of the acid-treated TCP groups were not significantly different from the control TCP group (p > 0.05). There was also no significant difference between the HF-treated TCP and TCP-NoPM groups (p > 0.05) after 1 year, all exhibiting greater than 10 MPa tensile bond strength. It is suggested that acidic pretreatment of the ceramic surface does not improve the durability of the dual-cure resin cement/silicon oxide ceramic bond when an acidic phosphate monomer is present as an activator in a ceramic primer.     

Fracture toughness of human dentin

The purpose of this study was to determine the fracture toughness (K(IC)) of human dentin and to test the null hypothesis that K(IC) is not affected by the orientation of dentinal tubules relative to the plane of crack propagation. Triangular prisms (4 x 4 x 4 x 8 mm) were obtained from human molars and tested using the notchless triangular prism (NTP) specimen K(IC) test. Dentin prisms were prepared so that the plane of crack propagation would have three different orientations relative to the orientation of dentinal tubules: perpendicular (PE), parallel aligned (PAA), and parallel transverse (PAT). The prepared specimens were secured in the specimen holder and loaded in tension until fracture or crack arrest. The maximum load recorded was used to calculate K(IC). There was no significant difference between the K(IC) of PAA specimens (1.97 +/- 0.17 MPa/m(1/2)) and PAT (2.02 +/- 0.18 MPa/m(1/2)). The K(IC) for the PE specimens (1.13 +/- 0.36 MPa/m(1/2)) was significantly lower. The SEM images of the fractured surfaces showed distinct differences that were correlated with the determined K(IC) values. The fractured surfaces of PAA and PAT specimens were rougher compared to PE specimens. Both the hyper mineralized peritubular dentin and the orientation of collagen fibrils surrounding the tubules could be responsible for the significant differences in K(IC). The results of this study identified a significant anisotropy of dentin with respect to its K(IC).