Effect of smear layer characteristics on dentin bonding durability of HEMA-free and HEMA-containing one-step self-etch adhesives

The purpose of this study was to evaluate the effect of smear layer characteristics on the dentin bonding durability of HEMA-free and HEMA-containing one-step self-etch adhesives. Xeno V (XV; HEMA-free), G BOND PLUS (GB; HEMA-free) and Clearfil S(3 )Bond (S(3); HEMA-containing), were applied to dentin surfaces prepared with either #180- or #600-grit SiC paper according to manufacturers' instructions. Bond strengths to dentin were determined using μTBS test after 24-hour, 6-month, and 1-year water storage. In addition, nanoleakage evaluation was performed using an SEM. The smear layer characteristics affected water-tree nanoleakage formation in the adhesive layers of XV and GB, which contributed to a reduction in μTBS after 6-month water storage, while the characteristics did not affect the μTBS of S(3). However, regardless of the smear layer characteristics, 1-year water storage significantly reduced the μTBS of all the adhesives and was associated with an increase in failures at the adhesive-composite interface.     

Effect of smear layer deproteinizing on resin–dentine interface with self-etch adhesive

Objectives

This study aimed to investigate deproteinizing effect of sodium-hypochlorite (NaOCl) and mild acidic hypochlorous-acid (HOCl) pretreatment on smear layer-covered dentine and to evaluate their effects on morphological characteristics of resin–dentine interface with self-etch adhesive.

Methods

Human coronal-dentine discs with standardized smear layer were pretreated with 6% NaOCl or 50 ppm HOCl for 15 s or 30 s. Their deproteinizing effects at the treated smear layer-covered dentine surfaces were determined by the measurement of amide:phosphate ratio using ATR-FTIR analysis. In addition, using TEM, micromorphological alterations of hybridized complex and nanoleakage expression were evaluated at the interface of a self-etch adhesive (Clearfil SE Bond) to the pretreated dentine surface with or without subsequent application of a reducing agent (p-Toluenesulfinic acid salt; Accel^®).

Results

Both pretreatments of NaOCl and HOCl significantly reduced the amide:phosphate ratio as compared with the no-pretreated group (p < 0.05), coincident with the elimination of the hybridized smear layer on their bonded interfaces. Nanoleakage within the hybrid layer was found in the no-pretreated and NaOCl-pretreated groups, whereas the subsequent reducing agent application changed the reticular nanoleakage to spotted type. HOCl-pretreated groups showed less nanoleakage expression in a spotted pattern, regardless of reducing agent application.

Conclusions

NaOCl and HOCl solutions could remove the organic component on the smear layer-covered dentine, which could eliminate the hybridized smear layer created by self-etch adhesive, leading to the reduction of nanoleakage expression within hybrid layer.

Clinical significance

Smear layer deproteinizing could modify dentine surface, giving an appropriate substrate for bonding to self-etch adhesive system.     

Two-year bond strengths of "all-in-one" adhesives to dentine

Objectives

To test the long-term in vitro bonding performance of “all-in-one” self-etch adhesives to dentine.

Methods

Adper Prompt (3M ESPE), Bond Force (Tokuyama), Brush &; Bond (Parkell), iBond Self Etch (Heraeus Kulzer), OptiBond All-In-One (Kerr), and Xeno IV (Dentsply Caulk) were tested. The two-step self-etch adhesive Clearfil SE Bond (Kuraray) served as the control. Extracted human teeth were assigned to groups after creation of smear layer on occlusal dentine. Adhesives were applied according to manufacturers’ instructions, and resin composite (Filtek Z250, 3M ESPE) build-ups were placed. The bonded specimens were sectioned into beams after 24 h of storage in water. Microtensile bond strengths (μTBS) was determined at baseline, and following one and two years of water storage using an EZ-Test device (Shimadzu). Representative specimens were examined under field emission scanning electron microscope. Fracture mode was recorded. The data were analyzed using linear mixed effects and least square means analyses. The significance level was set at 0.01 for the pairwise comparisons and at 0.05 for the overall model effects.

Results

The mean μTBS decreased significantly over time for Adper Prompt, iBond Self Etch, and OptiBond All-In-One. After two years of water ageing, Bond Force, Brush &; Bond, OptiBond All-In-One, and Xeno IV had mean μTBS values not statistically different from Clearfil SE Bond.

Conclusions

After two years of water ageing, Clearfil SE Bond outperformed two of six all-in-one adhesives. That indicates that the composition of the adhesives rather than their application approach is accountable for their performance.

Clinical significance

Despite the data available suggesting that most all-in-one adhesives are severely affected by hydrolytic degradation, results of the present in vitro study suggest that some may perform as well as the clinically proven Clearfil SE Bond in the longer term.     

Smear layer-deproteinizing improves bonding of one-step self-etch adhesives to dentin

Objectives

Smear layer deproteinizing was proved to reduce the organic phase of smear layer covered on dentin surface. It was shown to eliminate hybridized smear layer and nanoleakage expression in resin–dentin bonding interface of two-step self-etch adhesive. This study aimed to investigate those effects on various one-step self-etch adhesives.

Bonding effectiveness of two contemporary self-etch adhesives to enamel and dentin

Objectives

Among contemporary adhesives, self-etch adhesives have been adopted by general practitioners for routine adhesive restorative purposes, mainly because of their ease of use. However, many versions that differ for their clinical application procedure, pH, number of components, etc., are currently available on the market. The purpose of this study was to determine the bonding effectiveness of two new self-etch adhesives (Adper Easy Bond and Adper ScotchBond SE, 3M ESPE) to enamel and dentin using a micro-tensile bond strength (μTBS) protocol and to characterise the interfacial ultra-structure at enamel and dentin using transmission electron microscopy (TEM).

Methods

The adhesives were applied onto coronal human enamel and dentin surfaces and built up with the micro-hybrid resin composite Z100 (3M ESPE). The ‘gold-standard’ two-step self-etch adhesive Clearfil SE Bond (Kuraray) served as control. Specimens were sectioned to sticks and trimmed at the interface to a cylindrical hour-glass shape (‘trimmed’ micro-specimens). Non-demineralized and demineralized TEM sections through the adhesive-dentin/enamel interface were prepared by ultra-microtomy.

Results

The μTBS of the two self-etch adhesives to enamel was statistically significantly lower than that of the control. To dentin, the μTBS of Adper Easy Bond was significantly lower than that of Adper ScotchBond SE and the control. TEM showed a tight interface to enamel for all three self-etch adhesives. A relatively thick, completely demineralized and acid-resistant hybrid layer was formed at dentin by Adper ScotchBond SE, whereas the interaction of Adper Easy Bond was much shallower, and comparable to that of so-called ‘ultra-mild’ self-etch adhesives. Some degree of spot- and cluster-like nano-leakage was observed for both adhesives, but did not differ in extent and form from that observed for the control.

Conclusions

Although the new two self-etch adhesives revealed a tight interaction at both enamel and dentin, their bond strength to both tooth tissues was generally lower than that of the control adhesive. Nevertheless, their bonding effectiveness appears in line with other simplified self-etch adhesives.     

Bonding performance of universal adhesives in different etching modes

Objectives

The aim of this study was to compare the microtensile bond strength (μTBS) and resin penetration into dentine of three universal adhesives (UAs) applied in two different etching modes (i.e. self-etch or etch-and-rinse). The effect of thermocycling on the μTBS was also evaluated.

Methods

The occlusal third of sound human molars was removed and the exposed surfaces were treated with three UAs (Futurabond Universal, Scotchbond Universal Adhesive and All-Bond Universal) in self-etch or etch-and-rinse mode. Two one-step self-etch adhesives (Futurabond DC and Futurabond M) were applied on additional teeth as reference. After composite build up, the specimens were stored for 24 h in distilled water at 37 °C or thermocycled for 5000 cycles. Composite/dentine beams were prepared (1 mm²) and μTBS test was performed. Data was analyzed using three-way ANOVA and Tukey's test (α = 0.05). One additional tooth was prepared for each group for evaluation of infiltration ability into dentine by dyeing the adhesives with a fluorochrome (Rhodamine B). After longitudinal sectioning, the generated interfaces were examined under confocal laser scanning microscopy.

Results

The addition of an etching step did not significantly affect the μTBS of none of the UAs, when compared to their self-etch application mode. All pre-etched specimens showed considerably longer resin tags and thicker hybrid layers. Thermocycling had no significant effect on the μTBS of the UAs.

Conclusions

Application of an etching step prior to UAs improves their dentine penetration, but does not affect their bond strength to dentine after 24 h or after thermocycling for 5000 cycles.

Clinical significance

Similar bond strength values were observed for the UAs regardless of application mode, which makes them reliable for working under different clinical conditions.     

Adhesive performance of a multi-mode adhesive system: 1-Year in vitro study

Objectives

The aim of this study was to investigate the adhesive stability over time of a multi-mode one-step adhesive applied using different bonding techniques on human coronal dentine. The hypotheses tested were that microtensile bond strength (μTBS), interfacial nanoleakage expression and matrix metalloproteinases (MMPs) activation are not affected by the adhesive application mode (following the use of self-etch technique or with the etch-and-rinse technique on dry or wet dentine) or by ageing for 24 h, 6 months and 1 year in artificial saliva.

Methods

Human molars were cut to expose middle/deep dentine and assigned to one of the following bonding systems (N = 15): (1) Scotchbond Universal (3M ESPE) self-etch mode, (2) Scotchbond Universal etch-and-rinse technique on wet dentine, (3) Scotchbond Universal etch-and-rinse technique on dry dentine, and (4) Prime&Bond NT (Dentsply De Trey) etch-and-rinse technique on wet dentine (control). Specimens were processed for μTBS test in accordance with the non-trimming technique and stressed to failure after 24 h, 6 months or 1 year. Additional specimens were processed and examined to assay interfacial nanoleakage and MMP expression.

Results

At baseline, no differences between groups were found. After 1 year of storage, Scotchbond Universal applied in the self-etch mode and Prime&Bond NT showed higher μTBS compared to the other groups. The lowest nanoleakage expression was found for Scotchbond Universal applied in the self-etch mode, both at baseline and after storage. MMPs activation was found after application of each tested adhesive.

Conclusions

The results of this study support the use of the self-etch approach for bonding the tested multi-mode adhesive system to dentine due to improved stability over time.

Clinical significance

Improved bonding effectiveness of the tested universal adhesive system on dentine may be obtained if the adhesive is applied with the self-etch approach.     

A randomized controlled 5-year prospective study of two HEMA-free adhesives,a 1-step self etching and a 3-step etch-and-rinse,in non-carious cervical lesions

Objective

The aim of this study was to evaluate the 5 year clinical dentin bonding effectiveness of two HEMA-free adhesives in Class V non-carious cervical lesions.

Material and methods

A total of 169 Class V restorations were placed in 67 patients with a self-etching adhesive (G-Bond; 67), a 3-step HEMA and TEGDMA free etch-and-rinse (cfm; 51) and a control HEMA-containing etch-and-rinse adhesive (XP Bond; 51) in non-carious cervical lesions without intentional enamel involvement. The restorations were evaluated at baseline and yearly during a 5 year follow-up with modified USPHS criteria. Dentin bonding efficiency was determined by the percentage of lost restorations.

Results

During the 5 years, 159 restorations could be evaluated. Good short time dentin retention was observed for the three adhesives, there all adhesives fulfilled at 18 months the full acceptance ADA criteria. At 5 years a cumulative number of 22 lost restorations (13.8%) was observed. The HEMA-free adhesives showed significantly higher dentin retention compared to the HEMA-containing one. Loss of retention was observed for 5 G-Bond (7.9%), 4 cfm (8.3%) and 13 XP Bond (27.1%) restorations (p < 0.05). No post-operative sensitivity was reported by the participants. No secondary caries was observed.

Significance

The durability in non-carious cervical lesions of the HEMA-free adhesives was successful after 5 years. Despite concerns which have been raised, showed the 1-step SEA one of the best reported clinical dentin bonding effectiveness.     

Influence of different smear layers on bond durability of self-etch adhesives

Objective

The purpose of this study was to determine the influence of different smear layers on enamel and dentin bond durability of various types of self-etch adhesives.

Chemical interaction of 10-MDP (methacryloyloxi-decyl-dihydrogen-phosphate) in zinc-doped self-etch adhesives

Objectives

Zinc-doped dentine adhesives have been recently advocated to interfere with metallo-proteinases-mediated collagen degradation. Nevertheless, there is a little information about the effects of zinc ions on the chemical interaction of self-etch functional monomers to dentine. The aim of this study was to assess if the inclusion of zinc into the primers of self-etch adhesives containing MDP (10-methacryloyloxi-decyl-dihydrogen-phosphate) may interfere with their chemical interaction to calcium/dentine.

Methods

Caries-free human molars were bonded using two commercial self-etching adhesives [Clearfil SE bond (CSE) and S3 bond (S3)] doped with zinc nitrate and submitted to microtensile bond strength (μTBS) and interface nanoleakage evaluation. Moreover, MDP was synthesised to evaluate the chemical interaction with calcium/dentine through atomic absorption spectroscopy (AAS) and SEM-EDX in the presence or absence of zinc ions.

Results

AAS showed increasing formation of MDP–zinc rather than MDP–calcium salts (p = 0.002) in the presence of zinc. SEM-EDX confirmed the formation of zinc-rich phosphate deposits that were probably responsible for the significant reduction in μTBS and increased interfacial nanoleakage attained with zinc-doped CSE and S3.

Conclusion

These outcomes demonstrated that the excessive presence of zinc ions may jeopardise the bonding performance of MDP-containing self-etch adhesives.     

Improving the effect of NaOCl pretreatment on bonding to caries-affected dentin using self-etch adhesives

Objective

To evaluate the effect of sodium hypochlorite pretreatment on adhesion to normal and caries-affected dentin using self-etch adhesives.

Methods

Forty extracted human molars with coronal carious lesions were used in this experiment. The occlusal dentin surfaces including the caries-affected dentin in each group were treated as follows: group 1, rinsed with water; group 2, treated with 6% NaOCl for 15 s; group 3, treated with 6% NaOCl for 30 s; group 4, application with Accel for 30 s after NaOCl-30 s pretreatment. After rinsing with water and air-drying, the treated dentin surfaces were applied with self-etch systems (Bond Force and Clearfil Protect Bond) according to the manufacturers’ instructions, and built-up with resin composite. After 37 °C water storage for 24 h, the bonded normal or caries-affected dentin areas were isolated to create an hourglass configuration with a cross-sectional area of approximately 1 mm². The specimens were subjected to tensile stress at a cross-head speed of 1.0 mm/min.

Results

NaOCl-15 s pretreatment significantly improved the μTBS of both self-etch adhesives to caries-affected dentin, while the 30 s pretreatment did not affect them. For normal dentin, NaOCl-30 s pretreatment significantly reduced the μTBS of both self-etch adhesives although the 15 s pretreatment did not alter them. Furthermore, the application of Accel with a reducing effect increased the μTBS to normal and caries-affected dentin treated with NaOCl for 30 s.

Conclusions

The effects of NaOCl pretreatment on bonding of both self-etch adhesives were dependent upon type of dentin (normal and caries-affected dentin) and the treatment time.     

An in vitro evaluation of microtensile bond strengths of two adhesive bonding agents to residual dentine after caries removal using three excavation techniques

Objectives

To assess amounts of residual dentine retained after using three excavation techniques; the microtensile bond strengths (μTBS) to residual dentine, comparing etch-rinse vs. self-etching adhesives.

Methods

42 carious molars were subdivided (N = 21) dependent upon adhesive/composite system (Adper Scotchbond 1XT and Filtek Supreme vs. Filtek Silorane adhesive and composite). Dividing into three (N = 7), dependent upon caries excavation technique employed (hand vs. chemo-mechanical: Carisolv™ gel vs. experimental enzymatic gel (SFC-V)), caries removal was assessed using visual/tactile criteria and in situ autofluorescence (AF) confocal fibre-optic micro-endoscopy (CFOME). Post-restoration/four-week hydrated storage, four 0.9 mm² beams per tooth underwent μTBS testing/microscopic analysis of fractured surfaces. Three cavities from each excavation group were analysed using SEM.

Results

SEM revealed surface roughness with smear layer occluding tubule orifices in hand-excavated samples and a reduced, variable smear layer for both chemo-mechanical systems. CFOME AF assessment indicated hand excavation left sound dentine, Carisolv™ left affected dentine and SFC-V slightly under-prepared clinically. Mean μTBS values from etch-rinse samples (27 MPa (SD 3.9), hand; 22 MPa (SD 5.1), Carisolv™; 26 MPa (SD 4.4), SFC-V) showed statistical differences between hand and Carisolv™ groups. Mean μTBS data for self-etch samples (22 MPa (SD 3.3), hand; 27 MPa (SD 6.1), Carisolv™; 25 MPa (SD 4.7), SFC-V) showed significant differences between hand and Carisolv™, and hand vs. SFC-V. Failure loci distribution in etch-rinse samples was between dentine–adhesive, within adhesive and within composite whereas self-etch samples exhibited failure predominantly between adhesive and composite.

Conclusions

Data indicated that all null hypotheses were disproved.     

Long-term evaluation of water sorption and ultimate tensile strength of HEMA-containing/-free one-step self-etch adhesives

Objective

The objective of this study was to evaluate the water sorption (Wsp) and ultimate tensile strength (UTS) of HEMA-containing/free one-step self-etch adhesives after long-term water-storage.

Methods

Three HEMA-containing one-step self-etch adhesives (Bond Force (BF), Clearfil S³ Bond (S3) and OptiBond All-In-One (OP)), and one HEMA-free one-step self-etch adhesive, G Bond (GB) was used. After the solvents of each adhesive were evaporated, polymerised adhesive disks and dumbbell-shaped specimens of thirty-two each were prepared and divided into four groups of 14-, 90-, 180- and 360-day water-storage. After immersion in water for the designated storage periods, the disks were subjected to measurement of Wsp, and the dumbbell-shaped specimens were subjected to measurement of UTS. The data of Wsp and UTS were statistically analysed using a two-way ANOVA and Bonferroni test.

Results

Wsp of BF, S3 and OP increased over time, whereas for GB, there were no significant differences in Wsp among all the storage periods. Wsp of GB was lower than those of BF, S3 and OP in each period. The UTS of BF, S3 and OP decreased over time, whereas for GB, there were no significant differences in UTS among all storage periods. The highest UTS was initially seen in BF > GB = S3 = OP, and after 360-day water-storage, seen in BF = GB > OP = S3.

Conclusions

For the HEMA-containing adhesives, Wsp increased and UTS decreased over time. On the other hand, for the HEMA-free adhesive, Wsp and UTS did not significantly change even after 360-day water-storage.     

Monomer-to-polymer conversion and micro-tensile bond strength to dentine of experimental and commercial adhesives containing diphenyl(2,4,6-trimethylbenzoyl)phosphine oxide or a camphorquinone/amine photo-initiator system

Objectives

To compare the degree of conversion (DC) of adhesives initiated by diphenyl(2,4,6-trimethylbenzoyl)phosphine oxide (TPO) or a camphorquinone/tertiary amine system (CQ/Amine) as well as their ‘immediate’ micro-tensile bond strength (μTBS) to bur-cut dentine.

Methods

DC of Scotchbond Universal (‘SBU’; 3M ESPE), its experimental counterpart containing TPO as photo-initiator system, an experimental G-aenial Bond (‘Ga-B’; GC) adhesive formulation, and an experimental LUB-102 adhesive formulation (‘LUB’, Kuraray Noritake), containing as photo-initiatior system either 2 wt% CQ along with 2 wt% tertiary amine (‘SBU_CQ/Amine’; ‘Ga-B_CQ/Amine’; ‘LUB_CQ/Amine’), or 2 wt% TPO (‘SBU_TPO’; ‘Ga-B_TPO’; ‘LUB_TPO’), was determined using Fourier-transform infrared spectroscopy (FTIR), after being cured with a dual-wavelength light-curing unit (bluephase 20i, Ivoclar Vivadent). The same adhesive formulations were applied to bur-cut mid-coronal dentine of intact human molars, and subjected to a μTBS test after 1-week water storage. Besides being applied following a self-etch (SE) application mode, the adhesive formulations SBU_CQ/Amine and SBU_TPO were also applied following an etch-and-rinse (E&R) mode, this both for DS and μTBS measurement.

Results

No significant difference in DC was found for any of the adhesive formulations, except for SBU_CQ/Amine_SE and SBU_TPO_SE. For both SBU formulations, a significantly higher DC was reached for the E&R than the SE approach. Regarding μTBS, no significant differences were recorded, except for the significantly higher μTBS measured for SBU_CQ/Amine_E&R and SBU_TPO_E&R.

Conclusions

In self-etch adhesives, the photo-initiator TPO may be used instead of CQ/Amine. The curing and ‘immediate’ bonding efficiency depended on the application protocol (E&R versus SE), but not on the photo-initiator system.

Clinical significance

The photo-initiator TPO may be used in self-etch adhesives instead of CQ/Amine with similar curing and ‘immediate’ bonding efficiency.     

Solvent composition of one-step self-etch adhesives and dentine wettability

Objectives

Our aim was to determine the wettability of dentine by four commercial self-etch adhesives and evaluate their spreading rate on the dentine surface. Any correlation with chemical composition was sought, particularly with the amount of solvent or HEMA present in the adhesive. The adhesives used were AdheSE One, Optibond All.In.One, Adper Easy Bond and XenoV.

Methods

Chemical compositions were determined by proton nuclear magnetic resonance (NMR) spectroscopy of the adhesives dissolved in dimethylsulfoxide. Apparent contact angles for sessile drops of adhesives were measured on dentine slices as a function of time for up to 180 s. The water contact angles were determined for fully polymerised adhesives.

Results

All adhesives were water-based with total solvent contents ranging from 27% to 73% for HEMA-free adhesives, and averaging 45% for HEMA containing adhesives. The contents in hydrophobic groups decreased as water contents increased. No differences were found in the adhesive contact angles after 180 s even though the spreading rates were different for the products tested.

Conclusion

Water contact angles differed significantly but were not correlated with HEMA or solvent presence. Manufacturers use different approaches to stabilise acid co-monomer ingredients in self-etch adhesives. Co-solvents, HEMA, or acrylamides without co-solvents are used to simultaneously etch and infiltrate dentine. A large proportion of water is necessary for decalcification action.     

Effect of application mode on interfacial morphology and chemistry between dentine and self-etch adhesives

Objective

To investigate the influence of application mode on the interfacial morphology and chemistry between dentine and self-etch adhesives with different aggressiveness.

Methods

The occlusal one-third of the crown was removed from un-erupted human third molars, followed by abrading with 600 grit SiC under water. Rectangular dentine slabs were prepared by sectioning the tooth specimens perpendicular to the abraded surfaces. The obtained dentine slabs were treated with one of the two one-step self-etch adhesives: Adper Easy Bond (AEB, pH ∼ 2.5) and Adper Prompt L-Pop (APLP, pH ∼ 0.8) with (15 s, active application) or without (15 s, inactive application) agitation. The dentine slabs were fractured and the exposed adhesive/dentine (A/D) interfaces were examined with micro-Raman spectroscopy and scanning electron microscopy (SEM).

Results

The interfacial morphology, degree of dentine demineralization (DD) and degree of conversion (DC) of the strong self-etch adhesive APLP showed more significant dependence on the application mode than the mild AEB. APLP exhibited inferior bonding at the A/D interface if applied without agitation, evidenced by debonding from the dentine substrate. The DDs and DCs of the APLP with agitation were higher than those of without agitation in the interface, in contrast to the comparable DD and DC values of two AEB specimen groups with different application modes. Raman spectral analysis revealed the important role of chemical interaction between acid monomers of self-etch adhesives and dentine in the above observations.

Conclusion

The chemical interaction with dentine is especially important for improving the DC of the strong self-etching adhesive at the A/D interface. Agitation could benefit polymerization efficacy of the strong self-etch adhesive through enhancing the chemical interaction with tooth substrate.     

Active application improves the bonding performance of self-etch adhesives to dentin

Objectives

To evaluate the effect of application method on immediate and 6-month resin–dentin microtensile bond strength (μTBS) and nanoleakage (NL) of three one-step self-etch adhesives systems (Clearfil S³ Bond (S3), Xeno III (XE) and Adper Prompt L-Pop (AD)).

Methods

The oclusal enamel of 30 human molar was removed in order to expose a flat dentin surface. The adhesives were applied under two modes: inactive (IN) or active (AC) application. After light-curing (600 mW/cm² for 10 s), composite buildups were constructed incrementally and sectioned to obtain bonded sticks (0.8 mm²) to be tested in tension immediately (IM) or after 6 months (6M) of water storage. For NL, three bonded sticks from each tooth at each time were coated with nail varnish, placed in silver nitrate and polished down with SiC paper. The μTBS data were submitted to a two-way ANOVA and Tukey’s test for each adhesive (α = 0.05).

Results

The AC showed higher μTBS to dentin when compared to IN in both periods of time (p = 0.001). Only for AD, lower μTBS was seen after 6M for IN and AC techniques. XE and S3 adhesives applied under IN showed a higher amount of silver penetration throughout the hybrid layer. Low silver nitrate deposition was seen for these adhesives under AC. After 6M, AD showed a higher amount of silver nitrate uptake under IN and AC techniques.

Conclusions

AC improves the bonding performance of all one-step self-etch adhesive systems tested regardless of the time and this tendency was maintained over time.     

Hydrolytic degradation of the resin–dentine interface induced by the simulated pulpal pressure,direct and indirect water ageing

Objectives

The aim of this study was to compare the hydrolytic effects induced by simulated pulpal pressure, direct or indirect water exposure within the resin–dentine interfaces created with three “simplified” resin bonding systems (RBSs).

Methods

A two-step/self-etching (CSE: Clearfil SE Bond), one-step/self-etching (S3: Clearfil S3) and etch-and-rinse/self-priming (SB: Single-bond 2) adhesives were applied onto dentine and submitted to three different prolonged (6 or 12 months) ageing strategies: (i) Simulated Pulpal Pressure (SPP); (ii) Indirect Water Exposure (IWE: intact bonded-teeth); (iii) Direct Water Exposure (DWE: resin–dentine sticks). Control and aged specimens were submitted to microtensile bond strength (μTBS) and nanoleakage evaluation. Water sorption (WS) survey was also performed on resin disks. Results were analysed with two-way ANOVA and Tukey's test (p < 0.05).

Results

The μTBS of CS3 and SB dropped significantly (p < 0.05) after 6 months of SPP and DWE. CSE showed a significant μTBS reduction only after 12 months of DWE (p = 0.038). IWE promoted no statistical change in μTBS (p > 0.05) and no evident change in nanoleakage. Conversely, SPP induced a clear formation of “water-trees” in CS3 and SB. WS outcomes were CS3 > SB = CSE.

Conclusion

The hydrolytic degradation of resin–dentine interfaces depend upon the type of the in vitro ageing strategy employed in the experimental design. Direct water exposure remains the quickest method to age the resin–dentine bonds. However, the use of SPP may better simulate the in vivo scenario. However, the application of a separate hydrophobic solvent-free adhesive layer may reduce the hydrolytic degradation and increase the longevity of resin–dentine interfaces created with simplified adhesives.     

Bond strengths, degree of conversion of the cement and molecular structure of the adhesive-dentine joint in fibre post restorations

Objectives

Because fibre post restorations are influenced by multiple factors such as the types of bonding materials, the dentine region and the time under moist exposure, this study sought to determine the bond strength of endodontic restorations and its relation to the degree of conversion of the cement layer and the molecular structure of the dentine-bonded joints.

Methods

The performance of 2 etch-and-rinse (All-Bond 2 and One-Step Plus) and 2 self-etch (Clearfil SE Bond and Xeno III) adhesives at post spaces regions, after 7 d or 4 m, was evaluated. FRC Postec Plus posts were cemented to the root canal with a dual-cure resin cement (Duo-Link). Transverse sections of the tooth were subjected to push-out testing, to degree-of-conversion measurements and to hybrid layer evaluation through μ-Raman spectroscopy.

Results

Coronal bonding was higher than cervical and middle bonding. The hybrid layer was thicker for the etch-and-rinse systems, with thicknesses decreasing towards the middle region. The degree of conversion measured for the 3-step etch-and-rinse group after 4 m was significantly higher than that for the self-etching groups.

Conclusions

Although not totally stable at the adhesive–dentine interface, the 3-step etch-and-rinse adhesive in the coronal dentine provided the best bond strength, degree of conversion of the cement and hybrid layer thickness in post restorations, in both short- and long-term analyses.     

Slow progression of dentin bond degradation during one-year water storage under simulated pulpal pressure

Objectives

To evaluate the dentin bond durability of simplified adhesives after one-year (1 y) under water storage and simulated pulpal pressure.

Methods

Class I cavities were prepared in sixty human third molars with the pulpal wall located in mid-coronal dentin. The roots were cut off to expose the pulpal chamber, and the teeth were assembled in a pulpal pressure simulator device. A two-step etch-and-rinse adhesive (Single Bond 2/SB), a two-step self-etch adhesive (Clearfil SE Bond/CSE), a three-step self-etch adhesive (Adper Scotchbond SE/SSE) and three all-in-one adhesives (Adper Easy Bond/EB, Clearfil S³ Bond/S3 and Adhese One/AO) were applied according to manufacturer? instructions. No enamel pre-etching was used for the self-etch systems. The cavities were filled with a composite (Z250, 3M ESPE) in four to five horizontal increments and individually cured. Immediately after the final cure, pulpal pressure was set to 15 cm H₂O. After 24 h and 1 y under simulate pulpal pressure the teeth were cut following a ‘nontrimming’ microtensile test technique (n = 30) and tested in tension. Kruskall–Wallis and post hoc multiple comparisons were used at α = 0.05. Weibull statistics was applied to SB, CSE and EB. Fractographic analysis of debonded specimens was performed using scanning electron microscopy.

Results

At 24 h and 1 y periods, SB showed higher bond strength means than all the others adhesives tested. CSE was not statistically different from EB at 24 h and from EB and SB at 1 y. EB showed bond strength statistically higher than the other three self-etch adhesives, which were not statistically different from each other at 24 h. AO showed significantly lower bond strength than all tested materials after 1 y. For all adhesives the mean bond strength at 1 y were not statistically different from the values measured at 24 h (p > 0.05). Shifts in failure mode patterns and Weibull modulus decrease indicate some degree of bond degradation after the 1 y storage period.

Conclusion

One-year of simulated pulpal pressure did not affect dentin bond strength of simplified adhesives in Class I restorations. Signs of degradation were only revealed by fractographic analysis and reliability parameters.