Characterisation of resin-dentine interfaces by compressive cyclic loading

The aims of this in vitro study were to evaluate the ultra-morphological changes in resin-dentine interfaces after different amounts of thermomechanical load (TML), and to determine the corresponding microtensile bond strengths (microTBS). Enamel/dentine discs with a thickness of 2 mm were cut from 24 human third molars and bonded with four adhesives involving different adhesion approaches: Syntac (Ivoclar Vivadent; used as multi-step etch-and-rinse adhesive), Clearfil SE Bond (Kuraray; two-step self-etch adhesive), Xeno III (Dentsply DeTrey; mixed all-in-one self-etch primer adhesive system), and iBond (Heraeus Kulzer; non-mixed all-in-one self-etch adhesive). The resin-dentine discs were cut into beams (width 2 mm; 2 mm dentine, 2 mm resin composite) and subsequently subjected to cyclic TML using ascending amounts of mechanical/thermal cycles (20 N at 0.5 Hz of mechanical load and 5-55 degrees C of thermal cycles: for 0/0, 100/3, 1,000/25, 10,000/250, 100,000/2,500 cycles). Loaded specimens were either cut perpendicularly in order to measure microTBS (n=20; crosshead speed: 1 mm/min) or were immersed in an aqueous tracer solution consisting of 50 wt% ammoniacal silver nitrate and processed for ultra-morphological nanoleakage examination using transmission electron microscopy (TEM). microTBS were significantly decreased by increasing amounts of TML for all adhesives (p<0.05). Bond strengths after 0 vs. 100,000 thermomechanical cycles were: Syntac: 41.3/30.1 MPa; Clearfil SE Bond 44.8/32.5 MPa; Xeno III 27.5/13.7 MPa; iBond 27.0/6.2 MPa. Relatively early, a certain amount of nanoleakage was observed in all groups by TEM, which was more pronounced for Xeno III and iBond. The incidence of nanoleakage remained stable or was even reduced with increasing load cycles for all adhesives except iBond, where exact failure origins were detected within the adhesive and at the top of the hybrid layer.     

A challenge to the conventional wisdom that simultaneous etching and resin infiltration always occurs in self-etch adhesives

This study provided morphological evidence that discrepancies between the depth of demineralisation and the depth of resin infiltration can occur in some mild self-etch adhesives. Sound dentine specimens derived from extracted human third molars were bonded with 5 one-step and 5 two-step self-etch adhesives. One millimeter thick slabs containing the resin-dentine interfaces were immersed in 50 wt% aqueous ammoniacal silver nitrate and processed for TEM examination. A zone of partially etched but uninfiltrated dentine was identified beneath the hybrid layers in the milder versions of both one-step and two-step self-etch adhesives. This zone was characterised by the occurrence of silver deposits along the interfibrillar spaces of mineralised collagen fibrils. The silver infiltrated interfibrillar spaces were clearly identified from the one-step self-etch adhesives Xeno III, iBond, Brush&Bond and the experimental adhesive, and were thinner and only occasionally observed in the two-step self-etch adhesives Clearfil SE Bond and Clearfil Protect Bond. The more aggressive one-step and two-step adhesives that exhibit more abrupt transitions from completely demineralised to mineralised dentin were devoid of these silver-infiltrated interfibrillar spaces beneath the hybrid layers. Incomplete resin infiltration observed in some self-etch adhesives may be caused by the reduced etching potential of the acidic monomers toward the base of hybrid layers, or the presence of acidic but non-polymerisable hydrolytic adhesive components, creating potential sites for the degradation of the bonded created by these self-etch adhesives.     

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.     

Microtensile bond strength of etch and rinse versus self-etch adhesive systems

The aim of this study was to compare the microtensile bond strength of the etch and rinse adhesive versus one-component or two-component self-etch adhesives. Twelve intact human molar teeth were cleaned and the occlusal enamel of the teeth was removed. The exposed dentin surfaces were polished and rinsed, and the adhesives were applied. A microhybride composite resin was applied to form specimens of 4?mm height and 6?mm diameter. The specimens were sectioned perpendicular to the adhesive interface to produce dentin-resin composite sticks, with an adhesive area of approximately 1.4?mm(2). The sticks were subjected to tensile loading until failure occurred. The debonded areas were examined with a scanning electron microscope to determine the site of failure. The results showed that the microtensile bond strength of the etch and rinse adhesive was higher than that of one-component or two-component self-etch adhesives. The scanning electron microscope examination of the dentin surfaces revealed adhesive and mixed modes of failure. The adhesive mode of failure occurred at the adhesive/dentin interface, while the mixed mode of failure occurred partially in the composite and partially at the adhesive/dentin interface. It was concluded that the etch and rinse adhesive had higher microtensile bond strength when compared to that of the self-etch adhesives.     

Nanoleakage within the hybrid layer: a correlative FEISEM/TEM investigation

The aim of this study was to compare the nanoleakage patterns of the resin-dentin interfaces of three dentin bonding systems at both TEM and field emission in lens SEM (FEI-SEM) levels. A standardized smear layer was created with 180-grit silicon carbide paper (SiC) on dentin disks obtained from 18 noncarious human third molars. Specimens were randomly divided into three groups and bonded with a two-step total etching adhesive (Single Bond, SB), a two-step, self-etching adhesive (Clearfil SE BOND, SEB), and a one-step, self-etching adhesive (XENO III, XEIII). Nanoleakage was evaluated by using an ammoniacal silver-nitrate solution. Specimens were processed for TEM and FEI-SEM observation. The TEM of SB revealed silver deposits in adhesive and hybrid layers (HL). High-magnification FEI-SEM micrographs clearly identified these deposits as spherical clusters mainly associated with nonembedded collagen fibrils. TEM and FEI-SEM examination of SEB revealed some clusters of silver deposits within porosities and small channels of the HL. Additional silver deposits were observed between the peritubular dentin walls and the resin tags. XEIII revealed very fine and diffuse silver grains throughout the entire HL. SEM visualization of nanoleakage at a high level of resolution has not been previously described. FEI-SEM technology supported the TEM visualization with three-dimensional morphological data of the relations between the HL constituents and nanoleakage. The results of the present study confirm the hypothesis that both total- and self-etch adhesives are not able to fully infiltrate the dentin substrate.     

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.     

Ultramorphological analysis of resin-dentin interfaces produced with water-based single-step and two-step adhesives: nanoleakage expression

This study evaluated the nanoleakage patterns in bonded interfaces using two single-step, self-etching adhesives (Adper Prompt-AD, and One-up Bond F-OB), two two-step, self-etching primers (Clearfil SE Bond-CF, and Unifil Bond-UB), and one two-step, total-etch adhesive (Single Bond-SB). Dentin surfaces were bonded with the adhesive systems and stored in water at 37 degrees C for 1 week and 6 months. After storage periods, teeth were sectioned into 0.8 mm-thick slabs, coated with nail varnish except for the bonded interfaces, and immersed in ammoniacal AgNO(3) for 24 h. After immersion in photodeveloping solution, bonded sections were prepared and observed under a SEM using the backscattered electron mode. Undemineralized, unstained, epoxy resin-embedded sections were prepared for TEM. Nanoleakage patterns were qualitatively compared between periods. Nanoleakage was observed in all bonded specimens at both periods. CF and UB presented silver deposits predominantly restricted to the thin (0.5 microm) hybrid layer (HL) at both periods. Although no evident differences were observed in the nanoleakage pattern of UB at 7 days and 6 months, CF presented enlarged areas of silver impregnation after 6 months. SB presented accumulation of silver particles mostly within the HL at 7 days, which was intensified after 6 months. AD and OB presented massive silver accumulation within the HL and the overlying adhesive layer. No evident differences were noticed between storage periods. Silver impregnation increased for all adhesive systems from 7 days to 6 months, except for UB.     

Evaluation of the fatigue behavior of the resin-dentin bond with the use of different methods

The clinical performance of directly bonded resin composites is fundamentally dependent on durable adhesion to prevent gap formation over time. The goal of this investigation was to evaluate the effectiveness of various dentin adhesives by means of quasistatic and dynamic dentin bond strengths, and also to determine marginal and internal gap formation after loading in an artificial oral environment. Three hundred thirty human third molars were used within four weeks of extraction. Adhesives used were A.R.T. Bond, OptiBond FL, Scotchbond Multi-Purpose Plus, Single Bond, Prime & Bond NT, and One Up Bond F for bonding of one resin composite (Z 250). Buccal and lingual aspects of 90 teeth were ground flat to expose dentin, then resin composite cylinders were bonded. Initial bond strengths (n = 10) and adhesive fatigue limits (n = 20) were determined with the use of a shear test apparatus. One hundred eighty conical cavities were prepared into dentin discs and filled with the same materials. After 21 days of storage, initial push-out bond strengths (n = 10) and adhesive fatigue limits (n = 20) were measured. Sixty molars with MO cavities (n = 10) with margins below the cement-enamel junction were filled. Before and after thermomechanical loading (100000 x 50 N and 2500 x thermocycling between + 5 and + 55 degrees C), marginal gap formation and internal adaptation (only after loading) were analyzed under a SEM (x 200). The one-bottle systems showed higher shear bond strengths when evaluated statically and dynamically. However, cyclic fatigue push-out bond strengths resulted in higher values for older multistep systems. Marginal and internal gap analysis confirmed the results, in favor of older adhesive systems (p <.05; Mann-Whitney U test).     

Adhesion to chondroitinase ABC treated dentin

Dentin bonding relies on complete resin impregnation throughout the demineralised hydrophilic collagen mesh. Chondroitin sulphate-glycosaminoglycans are claimed to regulate the three-dimensional arrangement of the dentin organic matrix and its hydrophilicity. The aim of this study was to investigate bond strength of two etch-and-rinse adhesives to chondroitinase ABC treated dentin. Human extracted molars were treated with chondroitinase ABC and a double labeling immunohistochemical technique was applied to reveal type I collagen and chondroitin 4/6 sulphate distribution under field emission in-lens scanning electron microscope. The immunohistochemical technique confirmed the effective removal of chondroitin 4/6 sulphate after the enzymatic treatment. Dentin surfaces exposed to chondroitinase ABC and untreated specimens prepared on untreated acid-etched dentin were bonded with Adper Scotchbond Multi-Purpose or Prime and Bond NT. Bonded specimens were submitted to microtensile testing and nanoleakage interfacial analysis under transmission electron microscope. Increased mean values of microtensile bond strength and reduced nanoleakage expression were found for both adhesives after chondroitinase ABC treatment of the dentin surface. Adper Scotchbond Multi-Purpose increased its bond strength about 28%, while bonding made with Prime and Bond NT almost doubled (92% increase) compared to untreated specimens. This study supports the hypothesis that adhesion can be enhanced by removal of chondroitin 4/6 sulphate and dermatan sulphate, probably due to a reduced amount of water content and enlarged interfibrillar spaces. Further studies should validate this hypothesis investigating the stability of chondroitin 4/6 and dermatan sulphate-depleted dentin bonded interface over time.     

Micro-rotary fatigue of tooth-biomaterial interfaces

The bonding effectiveness of restorative materials to tooth tissue is typically measured statically. Clinically tooth/composite bonds are however subjected to cyclic sub-critical loads. Therefore, in vitro fatigue testing of dental adhesives should predict better the in vivo performance of adhesives. The objective of this study was to determine the fatigue resistance of two representative adhesives, a self-etch and an etch&rinse adhesive, bonded to enamel and dentin. Therefore, tooth/composite interfaces were cyclically loaded using a miniaturized version of a rotating beam fatigue testing device. Subsequently, the load at which 50% of the specimens fail after 10(5) cycles, was determined as the median micro-rotary fatigue resistance (microRFR). For both adhesives, the microRFR was about 30-40% lower than the corresponding micro-tensile bond strength (microTBS) to both enamel and dentin. Analysis of the fracture surfaces by Feg-SEM revealed typical fatigue fracture patterns. It is concluded that resin/tooth interfaces are vulnerable to progressive damage by sub-critical loads, with the 3-step etch&rinse adhesive being more resistant to fatigue than the 2-step self-etch adhesive.     

Nanoleakage and microshear bond strength in deproteinized human dentin

This study evaluated the influence of dentin deproteinization with NaOCl on the microshear bond strength (microSBS) and the nanoleakage patterns of three dentin bonding systems (DBS). Occlusal dentin surfaces, obtained from extracted noncarious human molars, were divided into two experimental groups, according to dentin surface treatment: Group I-37% H(3)PO(4)/15s and Group II-37% H(3)PO(4)/15s + 10% NaOCl/1 min. The dentin surfaces were bonded with one of the following DBS: Scotchbond Multipurpose-SBMP, Prime & Bond NT-PB and Clearfil SE Bond-SE. After 1 week storage in water at 37 degrees C, the specimens were subjected to the microSBS test. The data were analyzed by two-way ANOVA and Student-Newman-Keuls' test (p = 0.05). The nanoleakage was evaluated using scanning electron microscopy (SEM) in backscattered electron imaging regime. No significant difference in microSBS between dentin treatments was found for SBMP. For PB, microSBS increased after NaOCl dentin treatment. SE showed a reduction in microSBS in deproteinized specimens. SEM analysis showed different nanoleakage patterns for each DBS. Irrespective of dentin treatments, all SBMP specimens showed nanoleakage. SE did not show nanoleakage with the two dentin treatments. PB showed nanoleakage within the hybrid layer only in acid-etched specimens. The influence of dentin deproteinization was dependent on the dentin bonding system formulation.     

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.     

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.     

The effect of two configuration factors,time, and thermal cycling on resin to dentin bond strengths

Most in vitro testing of bonding systems is performed using specimens made in a mold with a low configuration (C) factor (ratio of bonded/unbonded surfaces) whereas clinically the C-factor is usually much greater. This study compared the effect of thermal cycling on the measured shear bond strength of 3M Single Bond dental adhesive bonded to dentin using molds with two different C-factors. The hypothesis was that neither C-factor nor thermal cycling would affect measured bond strengths. Resin composite was bonded to human dentin in cylindrical molds with an internal diameter of 3.2mm and either 1mm or 2.5mm deep. The 1mm deep molds had a C-factor of 2.2 and the 2.5mm deep molds had a C-factor of 4.1. Specimens were debonded either 10min after they had been bonded to dentin, or after they had been stored for 7 days in water at 37+/-1 degrees C, or after thermal cycling 5000 times for 7 days. Two-way ANOVA showed that overall both the C-factor and the storage condition had a significant effect on bond strength (p<0.001). There was a significant interaction (p<0.001) between the C-factor and how the specimens had been stored. The GLM/LSMEANS procedure with Sidak's adjustment for multiple comparisons showed that overall the specimens made in the mold with a high C-factor (4.1) had a lower bond strength than those that had been made in the mold with a lower (2.2) C-factor (p<0.001). Thermal cycling had a negative effect on the bond strength only for specimens made in molds with a C-factor of 4.1 (p<0.001).     

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.     

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.     

Adhesive layer properties as a determinant of dentin bond strength

The goal of this study is to evaluate the hypothesis that the properties of the resin adhesive might affect the microtensile bond strength (MTBS) of multibottle dental adhesive system. In order to alter the properties, the experimental resin adhesives containing 2,2-bis (4-2-hydroxy-3-methacryloyloxypropoxyphenyl)propane (Bis-GMA) and triethylene glycol dimethacrylate (TEGDMA) at various ratios were prepared. Degree of conversion immediately after curing (DC-immed), degree of conversion at 48 h after curing (DC-48h) of a thin coat of the experimental adhesives, the flexural strength (FS) of the bulk specimens made of the experimental adhesives, pH, viscosity at shear rate of 1 S(-1), and the microtensile bond strength (MTBS) values of the adhesives to dentin were investigated. The maximum MTBS and FS values of the resin adhesives were observed when the ratio of Bis-GMA/TEGDMA was 60/40. However, pH and viscosity values increased with increasing Bis-GMA content in the adhesives. When Bis-GMA content was more than 60 wt %, the viscosity increased exponentially and restricted the DC and FS, and accordingly decreased the bond strength. The stronger the resin adhesives were, the higher the bond strength to dentin could be obtained.     

Polycarboxylated microfillers incorporated into light-curable resin-based dental adhesives evoke remineralization at the mineral-depleted dentin

This study aimed at evaluating the remineralizing properties of three experimental light-curable resin-based dental adhesives containing tailored polycarboxylated microfillers. A co-monomers blend was firstly formulated and then mixed with each of the following microfillers: polycarboxylated bioactive glass (PBAG), polycarboxylated calcium silicates (PCS), and polycarboxylated calcium silicates-doped brushite (PDP). The three experimental and a filler-free control resins were applied onto 10% orthophosphoric acid treated dentin discs and light cured. The specimens were soaked in artificial saliva (AS) for 3, 7, and 14?days. Dentin mineral variation was monitored using attenuated total reflection-Fourier transform infrared (ATR-FTIR) and Raman spectroscopy. Confocal laser scanning microscopy (CLSM) was employed to observe the ultra-morphology/nanoleakage along the resin–dentin interface. The bonding ability and the durability of the resin–dentin bonds were investigated through microtensile bond strength (μTBS) test. ATR-FTIR and Raman showed a significant increase of the mineral matrix area ratio and phosphate peak intensity in specimens treated with the experimental resins within 14?days (p?p?>?0.05). Dentin treated using PBAG or PCS exhibited higher level of remineralization than the specimens in PDP group. CLSM showed reduction in nanoleakage, although the remineralization of the hybrid layer induced a significant drop in the μTBS after 3-month storage (p?相似文献   

Effect of light-cure time of adhesive resin on the thickness of the oxygen-inhibited layer and the microtensile bond strength to dentin

A thick oxygen-inhibited layer (OIL) on a cured adhesive layer (AL) is believed to result in both good adaptation of composite resin (CR) and high bond strength. A high degree of conversion (DC) of the AL is also needed for durable bonding. This study evaluated the hypothesis that increasing the DC by prolonging the light-curing time of adhesive bonding resin might decrease the bond strength of the adhesive to dentin because of the subsequent thinning of the OIL thickness. The OIL thickness and the DC of solvent-removed One Step and D/E bonding resin of All Bond 2 (Bisco, USA) were measured simultaneously with FT-NIR spectroscopy according to increasing light-cure times (10, 20, 30, and 60 s) so as to evaluate their effect on the microtensile bond strength. The bonded interfaces were evaluated using scanning electron microscopy. Excessive irradiation of light-curing adhesives increased the DC, but decreased the OIL thickness. When the OIL was significantly thin by curing the adhesives for 30 or 60 s, defects were observed at the interface between the AL and the CR, as well as at the interface between the AL and the hybrid layer. When the OIL was thick, free radicals from the overlying CR may have diffused into the unreacted monomer mixtures of the OIL, chemically connecting the cured AL and the newly curing composite. It was found that to obtain maximum dentin bond strength, light-curing adhesives should be cured for the irradiation time recommended by the manufacturer.     

Improvement of the bond strength of 4-META/MMA-TBB resin to collagen-depleted dentin

It has been reported that the tensile bond strength between the 4-META/MMA-TBB resin and dentin pretreated with 10% citric/3% ferric chloride solution decreased after immersion in water for 2 years. The current study investigated the effect of an experimental dentin conditioner on the bonding of 4-META/MMA-TBB resin to dentin after thermocycling. The experimental conditioner was an aqueous solution of 10% ascorbic acid and 5% ferric chloride (Exp). Human teeth were prepared to expose flat dentin surfaces. These were treated sequentially with 40% phosphoric acid, 10% sodium hypochlorite, and the experimental conditioner. A commercially available dentin conditioner, an aqueous solution of 10% citric/3% ferric chloride (10-3) was used for a control group. Stainless steel rods were bonded to the pretreated dentin surfaces with the use of the 4-META/MMA-TBB resin. Tensile bond strengths were determined after 0, 5,000, 10,000, 20,000 themocycles. All data were analyzed by ANOVA, and differences among groups were analyzed by Duncan's new multiple range test (n = 10, p < 0.05). The experimental group showed no significant decrease in bond strength through 20,000 thermocycles, while the control group exhibited significant decrease after 10,000 thermocycles. Mean bond strength of the experimental groups were significantly higher than those of the control group at both 10,000 and 20,000 thermocycles. A hybrid layer could not be identified in SEM micrographs of the experimental groups. 10-3-conditioned specimen SEMs displayed crack formation between the adhesive resin and a hybrid layer. The experimental dentin pretreatment improved the bond strength of a 4-META/MMA-TBB resin to human dentin compared to 10-3 treatment after thermocycling.