Interfacial chemistry of class II composite restoration: structure analysis

The gingival margins of class II composite restorations are particularly vulnerable to marginal leakage and secondary caries. In identifying the factors contributing to caries development, the molecular structure and differences in the structure at the proximal and gingival margins have been largely overlooked. The purpose of this study was to compare the molecular structure at the adhesive/dentin interface of the proximal and gingival walls of class II composite restorations. Class II preparations were cut in 12 unerupted third molars with a water-cooled high-speed dental handpiece. The prepared teeth were randomly selected for treatment with Single Bond (SB) + Z100 (3M). Teeth were restored, per manufacturer's directions, under humidity and temperature characteristic of the oral cavity. Restored teeth were kept in sterile Delbecco's phosphate saline for 48 h. The samples were sectioned occluso-gingivally and micro-Raman spectra were acquired at approximately 1.5-microm spatial resolution across the composite/adhesive/dentin interfaces. Samples were wet throughout spectral acquisition. Raman spectral characteristics at the proximal and gingival margins were distinctly different; the depth of demineralized dentin was 6-7 microm at proximal margin, 12-13 microm at gingival margin. SB adhesive penetrated the depth of demineralized dentin in a gradient at the proximal margin. The "single bottle" adhesive used in this study, gradually penetrated the depth of the demineralized dentin at the proximal margin but failed to infiltrate the depth at the gingival margin, leaving a thick exposed collagen layer.     

Enamel microhardness after in vitro demineralization and role of different restorative materials

This study aimed to evaluate the extension of enamel demineralization around the margin of restorations after immersion in cariogenic solution, in an attempt to define the role of new restorative materials in preventing secondary caries formation. For this purpose, enamel microhardness was measured. Twelve class V restorations in human extracted third molars were prepared in vitro and immersed in a demineralizing solution (lactic acid, pH 4.5) at 37 degrees C for 3 days to simulate the formation of secondary caries and its effect on the marginal integrity of composite restorations. The restorative systems tested in the study were Scotchbond 1 + Z 250 (group A), ABF + APX (group B), Fuji IX (group C), SE Bond + APX (group D), and Scotchbond 1 + F 2000 (group E). The microhardness was measured close to the margin of restoration (marginal exposed enamel), at 2.0 mm from the margin (exposed enamel), and at approximately 4 mm from the margin in a varnish-covered enamel area (protected enamel). Five measurements were made on each site at 20, 40, 60, 80, and 100 microm depth from the external enamel surface. Exposed enamel and marginal exposed enamel were greatly affected by the cariogenic solution, as confirmed by the high rate of demineralization. The marginal exposed enamel showed a higher rate of demineralization than the exposed enamel, as demonstrated by the lowest microhardness values. The materials that claimed fluoride release did not prevent any type of enamel marginal alteration. This study revealed that enamel close to the margin of restoration may be rapidly affected by secondary caries formation when immersed in a demineralizing-cariogenic solution and that fluoride-releasing materials are unable to reduce the marginal demineralization processes. These demineralization processes may be responsible for marginal secondary caries and for restoration failures.     

Marginal leakage of class V cavity preparations

Dentin-bonding materials, ferric oxylate (FO), addition reaction between N-phenylglycine and glycidyl methacrylate (NPG-GMA), and addition reaction product of pyromellitic acid dianhydride and 2-hydroxyethyl methacrylate (PMDM), were tested together for their ability to inhibit marginal leakage in Class V composite restorations in vitro. Sixteen experimental teeth were pretreated with FO, NPG-GMA, PMDM, and restored with composite. Sixteen control teeth were treated conventionally with composite. The teeth were then thermally cycled (5 and 55 degrees C) for 7 days, silver stained, and evaluated blindly for degree of marginal leakage on a scale of 0 (no leakage) to 7 (leakage into the pulp). The experimental group displayed significantly greater leakage values (p less than 0.01) than controls. The results of this study support the hypothesis that FO, NPG-GMA, and PMDM, together with composite inhibit marginal leakage.     

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.     

Hybrid layer seals the cementum/4-META/MMA-TBB resin interface

Although 4-META/MMA-TBB resin has adhesive properties to dentin, and has been clinically used for the bonding treatment of vertically fractured roots and apicoectomy, there has not been any investigation on the adhesion of 4-META/MMA-TBB resin to cementum. The purpose of this in vitro study was to evaluate the bonding and the sealing ability of 4-META/MMA-TBB resin to cementum. Bovine root cementum and dentin surfaces were treated with a citric acid and ferric chloride solution, and the 4-META/MMA-TBB resin was applied on the treated surfaces before testing. The microtensile bond strength and the leakage levels obtained for the cementum were almost equal to those for the dentin. In SEM and TEM observations, a hybrid layer approximately 2-3 microm in thickness was observed at the interface between the resin and the cementum. It is concluded that 4-META/MMA-TBB resin adhered to cementum via a hybrid layer on cementum, as previously reported for dentin.     

Influence of dentin substrates to simplify wet-bonding: a leakage-free and reliable tensile strength interface for long-lasting restorations

The wet-bonding procedure can be simplified by eliminating the primer. An aqueous mixture of 1% citric acid and 1% ferric chloride (1-1) was hypothesized as providing an easier dehydratable thinner substrate to which 4-META/MMA-TBB resin can adhere reliably. The 1-1 was applied for 10 s and rinsed off with water for 10 s. Demineralized dentin under four conditions was prepared before bonding to PMMA rod using 4-META/MMA-TBB resin: air-dried 10 s (D-NP); air-dried 10 s, primed 60 s with 5% 4-META in acetone (D-P); blotted dry 10 s (W-NP); blotted dry 10 s, primed 60 s (W-P). The tensile strengths (MPa) using mini-dumbbell specimens were 4.0 ± 2.4 for D-NP, 10.6 ± 5.4 for D-P, 38.3 ± 4.4 for W-NP, and 42.9 ± 3.3 for W-P. There was no significant difference between W-NP and W-P with cohesive failure in the dentin and the cured resin. In the wet groups, the hybridized dentin was stable against both HCl and NaOCl challenges. TEM examination and a leakage tests confirmed a perfect seal with a leakage-free interface of W-NP. These results suggest that this primer-less wet-bonding is promising method to protect the underlying intact dentin and pulp, thus providing long-lasting dental treatment.     

Enamel microhardness after in vitro demineralization and role of different restorative materials

This study aimed to evaluate the extension of enamel demineralization around the margin of restorations after immersion in cariogenic solution, in an attempt to define the role of new restorative materials in preventing secondary caries formation. For this purpose, enamel microhardness was measured. Twelve class V restorations in human extracted third molars were prepared in vitro and immersed in a demineralizing solution (lactic acid, pH 4.5) at 37°C for 3 days to simulate the formation of secondary caries and its effect on the marginal integrity of composite restorations. The restorative systems tested in the study were Scotchbond 1 + Z 250 (group A), ABF + APX (group B), Fuji IX (group C), SE Bond + APX (group D), and Scotchbond 1 + F 2000 (group E). The microhardness was measured close to the margin of restoration (marginal exposed enamel), at 2.0 mm from the margin (exposed enamel), and at approximately 4 mm from the margin in a varnish-covered enamel area (protected enamel). Five measurements were made on each site at 20, 40, 60, 80, and 100 μm depth from the external enamel surface. Exposed enamel and marginal exposed enamel were greatly affected by the cariogenic solution, as confirmed by the high rate of demineralization. The marginal exposed enamel showed a higher rate of demineralization than the exposed enamel, as demonstrated by the lowest microhardness values. The materials that claimed fluoride release did not prevent any type of enamel marginal alteration. This study revealed that enamel close to the margin of restoration may be rapidly affected by secondary caries formation when immersed in a demineralizing-cariogenic solution and that fluoride-releasing materials are unable to reduce the marginal demineralization processes. These demineralization processes may be responsible for marginal secondary caries and for restoration failures.     

Effects of a ferric chloride primer on collagen-depleted dentin bonding between tri-n-butylborane initiated self-curing resin and dentin

This study was designed to evaluate the micro-tensile bond strength between a carboxylic resin and dentin, when the dentin surface was modified with an experimental dentin primer. The three primers tested were ED primer II (ED), 0.3% ferric chloride aqueous solution (FE), and ED containing 0.3% ferric chloride (ED/FE). Three commercial dentin conditioners [40% phosphoric acid, 10% NaOCl, and 10% citric acid with 3% ferric chloride (10-3)] were also used. The coronal surfaces of extracted human molars were ground flat to dentin. The dentin surfaces were treated with phosphoric acid, NaOCl, or with one of the primers. The 10-3 was used without phosphoric acid or NaOCl as a control. A composite material rod was bonded to the dentin surface with 4-META/MMA-TBB resin. After 24-h immersion in 37 degrees C distilled water, 0.9 mm x 0.9 mm composite-dentin beams cut from the bonded specimens were stressed to failure in tension at 0.6 mm/min. The bond strengths were also evaluated after 5000 thermocycles. The bond strength of the group ED/FE was significantly higher than those of the 10-3, ED, and FE. After 5000 thermocycling, 10-3, ED and FE showed significant decrease in bond strength, although no significant decrease was seen for ED/FE. It was concluded that dentin surface treatment with phosphoric acid, NaOCl, and the ED/FE primer improved the bonding (p < 0.05) between 4-META/MMA-TBB resin and dentin, with or without thermocycling, while the bond strengths in the control group fell 34% following 5000 thermocycles.     

Microleakage and interfacial morphology of self-etching adhesives in class V resin composite restorations

The purpose of the study was to evaluate the marginal leakage of three adhesive systems in Class V resin composite restorations. Two adhesive systems containing acidic primers: Clearfil SE Bond (CSEB) and Etch & Prime 3.0 (E&P), were compared with a conventional water-based primer: Scotchbond Multipurpose Plus (SBMP). Class V cavities were made at the cementum-enamel junction of extracted human molars, which were then divided between three groups. One of the adhesive systems was applied to each group following manufacturers' instructions. Composite restorations were placed, light cured for 40 s, and polished. Specimens were then immersed in a solution of 2% basic fuchsin dye for 24 h. Longitudinal sections were obtained and studied with a stereomicroscope for assessment of the microleakage according to the degree of dye penetration (scale of 0-3). Data were analyzed by Kruskal-Wallis one-way ANOVA, Mann-Whitney tests, and the Wilcoxon matched-pairs signed rank test. Two specimens for each group were analyzed by scanning-electron microscopy (SEM). Bonded interfaces of dentin were also examined by transmission-electron microscopy (TEM). On enamel, there were no significant differences between the three groups. On dentin, CSEB showed the lowest dye penetration values among the three adhesive systems. SEM and TEM studies showed hybrid layer and resin tag formations in all groups.     

Strength and fluoride release characteristics of a calcium fluoride based dental nanocomposite

Secondary caries and restoration fracture remain the two most common problems in restorative dentistry. Release of fluoride ions (F) could be a substantial benefit because F could enrich neighboring enamel or dentin to combat caries. The objective of this study was to incorporate novel CaF(2) nanoparticles into dental resin to develop stress-bearing, F-releasing nanocomposite. CaF(2) nanoparticles, prepared in our laboratories for the first time, were combined with reinforcing whisker fillers in a resin. Flexural strength (mean+/-sd; n=6) was 110+/-11MPa for the composite containing 30% CaF(2) and 35% whiskers by mass. It matched the 108+/-19MPa of a stress-bearing, non-releasing commercial composite (Tukey's at 0.05). The composite containing 20% CaF(2) had a cumulative F release of 2.34+/-0.26mmol/L at 10weeks. The initial F release rate was 2mug/(hcm(2)), and the sustained release rate after 10weeks was 0.29mug/(hcm(2)). These values exceeded the reported releases of traditional and resin-modified glass ionomer materials. In summary, nanocomposites were developed with relatively high strength as well as sustained release of fluoride ions, a combination not available in current materials. These strong and F-releasing composites may yield restorations that can reduce the occurrence of both secondary caries and restoration fracture.     

A study on cytochrome c oxidoreductase for bonding a tri-n-butylborane-initiated luting agent to dentin.

The purpose of this study was to investigate the effectiveness of cytochrome c, an oxidoreductase, in terms of initiation of polymerization in dentin bonding. The efficacy of experimental dentin primers was evaluated via the bonding of a luting agent to dentin. The eight primers evaluated were cytochrome c aqueous solutions, four with 35 wt% 2-hydroxyethyl methacrylate (HEMA) and four without. The concentrations of cytochrome c in the primers were 0, 0.01, 0.1, and 1[corrected] micromol/g. The luting agent (Super-Bond C&B) consisted of methyl methacrylate (MMA), 4-methacryloyloxyethyl trimellitate anhydride (4-META), and tri-n-butylborane (TBB) initiator. Bovine dentin surfaces were flattened, etched with an aqueous solution of 10 wt% phosphoric acid, primed, and then bonded with stainless steel rods. After 1-day immersion in water, tensile testing revealed that the bond strength was influenced by the application of cytochrome c and HEMA. The maximum bond strength of 24.6 MPa was recorded with aqueous HEMA primer containing 10 micromol/g cytochrome c. This bonding technique, combining oxidoreductase with Super-Bond C&B, may potentially be applied for seating resin-bonded restorations.     

Adhesive bone cement both to bone and metals: 4-META in MMA initiated with tri-n-butyl borane

In order to develop a new bone cement which is expected to prevent loosening of a prosthesis by better adhesion, the cement composed of 4-methacryloyloxyethyl trimellitate anhydride (4-META) and methyl methacrylate (MMA) as monomers and tri-n-butyl borane (TBB) as an initiator was evaluated. The tensile bond strength between bone and metals adhered with 4-META/MMA-TBB cement was above 7 MPa. The values were higher than that with conventional bone cement (1 MPa) or MMA-TBB cement (2 MPa). Therefore, 4-META was effective for improving adhesion. When cohesive failure of the bone was observed with the scanning electron micrography after the tensile test, fracture occurred on the bone side below the interface between the bone and the 4-META/MMA-TBB cement. This result showed that the cement adhered tightly to both the bone and metals. Thus, it is concluded that the 4-META/MMA-TBB cement is useful as an adhesive bone cement.     

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.     

Fatigue crack propagation path across the dentinoenamel junction complex in human teeth

The human tooth structures should be understood clearly to improve clinically used restorative materials. The dentinoenamel junction (DEJ) plays a key role in resisting crack propagation in teeth. The aim of this study was to determine the fracture toughness of the enamel-DEJ-dentin complex and to investigate the influence of the DEJ on the fatigue crack propagation path across it by characterizing fatigue-fractured enamel-DEJ-dentin complexes using optical and scanning electron microscopy. The results of this study showed that the fracture toughness of the enamel-DEJ-dentin complex was 1.50 +/- 0.28 Mpa x m(1/2). Based on the results of this investigation, it was concluded that the DEJ complex played a critical role in resisting crack propagation from enamel into dentin. The DEJ complex is, approximately, a 100 to 150 microm broad region at the interface between enamel and dentin. The toughening mechanism of the DEJ complex may be explained by the fact that crack paths were deflected as cracks propagated across it. Understanding the mechanism of crack deflection could help in improving dentin-composite as well as ceramic-cement interfacial qualities with the aim to decrease the risk of clinical failure of restorations. Both can be viewed as being composed from a layer of material of high strength and hardness bonded to a softer but tougher substratum (dentin). The bonding agent or the luting cement layer may play the critical role of the DEJ in improving the strength of these restorations in clinical situations.     

口腔粘接新型材料——磷酸二氢(甲基丙烯酰氧癸)酯的合成与应用

以甲基丙烯酸、1,10-癸二醇和三氯氧磷为主要原料合成出了磷酸二氢(甲基丙烯酰氧癸)酯.用1HNMR、MS和31P-NMR对产物结构进行了表征确认.通过剪切强度的测试评价了磷酸二氢(甲基丙烯酰氧癸)酯对复合树脂与牙釉质、牙本质、钛合金、钴铬合金和高含金合金之间的粘接性能的影响.结果表明磷酸二氢(甲基丙烯酰氧癸)酯能够促进复合树脂与牙釉质、牙本质、钛合金、钴铬合金的粘接,剪切强度分别达到13.5、11.2、16.2和18.1 MPa.     

Adhesive bone cement containing hydroxyapatite particle as bone compatible filler.

Acrylic bone cement containing hydroxyapatite (HA) as a filler was developed using 4-methacryloyloxyethyl trimellitate anhydride (4-META) to promote adhesion both to bone and HA. The mechanical strengths of the cement did not decrease significantly with increasing HA in the cement by 4-META. However, strengths decreased with increasing HA content in the absence of 4-META. Scanning electron micrographic examination of fractured surfaces of the cement clearly showed that the HA particles adhered to the matrix resin when 4-META was added. Thus, it was important to maintain the original mechanical strengths for 4-META. The HA particles along the surface increased with increased HA content in the cement. The cement adhered to bone with a tensile bond strength was higher than 10 MPa.     

Strong composites of dimethylacrylates with 4-methacryloxyethyl trimellitic anhydride

Particles of a lithium aluminum silicate, which had been treated with a silane coupling agent, were centrifuged either in an adduct of bisphenol-A/glycidyl methacrylate (Bis-GMA) or in a mixture of Bis--GMA and methyl methacrylate. Polymerization was effected by heating with 2,5-dimethyl-hexane-2,5-dihydroperoxide. Flexural strength passed through an optimum value with increasing loading of the silicate. Inclusion of 4-methacryloxyethyl trimellitic anhydride, 4-META (5 wt % on monomer), increased the optimum flexural strength by about 20% (to 240 MPa). Evidence that 4-META increased the adhesion of filler particles to the polymeric matrix was obtained by examination of fracture surfaces.     

Exploration and preliminary clinical investigation of an adhesive approach for primary tooth restoration

The current study aims to investigate a suitable adhesive for primary tooth enamel. Shear bond strength (SBS) of primary teeth and the length of resin protrusion were analyzed using one-way ANOVA with Bonferroni multiple comparison tests after etching with 35% H₃PO₄. SBS and marginal microleakage tests were conducted with Single Bond Universal (SBU)/Single Bond 2 (SB2) adhesives with or without pre-etching using a nonparametric Kruskal-Wallis test. Clinical investigations were performed to validate the adhesive for primary teeth restoration using Chi-square tests. Results showed that the SBS and length of resin protrusion increased significantly with the etching time. Teeth in the SBU with 35% H₃PO₄ pre-etching groups had higher bond strength and lower marginal microleakage than those in the SB2 groups. Mixed fractures were more common in the 35% H₃PO₄ etched 30 s + SB2/SBU groups. Clinical investigations showed significant differences between the two groups in cumulative retention rates at the 6-, 12- and 18-month follow-up evaluations, as well as in marginal adaptation, discoloration, and secondary caries at the 12- and 18-month follow-up assessments. Together, pre-etching primary teeth enamel for 30 s before SBU treatment improved clinical composite resin restoration, which can provide a suitable approach for restoration of primary teeth.     

Development of self-etching primer comprised of methacrylamide, N-methacryloyl glycine

In order to develop a more effective self-etching primer, it is helpful to understand how a functional monomer conditions the surface of the teeth.

In this study, the reactivity by the carboxylic acid in the N-methacryloyl glycine (NMGly) on the calcium phosphate in hydroxyapatite or dentin was studied. The efficacy of the NMGly as a functional monomer for a self-etching primer was then examined.

Applying NMGly to both the enamel and dentin resulted in an increase in the bond strength of resin, since the carboxylic acid in the NMGly decalcified the calcium phosphate in the hydroxyapatite and dentin. The bond strength to dentin achieved was higher than with the enamel. This difference was most likely due to different enamel and dentin adhesion mechanisms.     

High-speed scanning ablation of dental hard tissues with a λ = 9.3 μm CO2 laser: adhesion, mechanical strength, heat accumulation, and peripheral thermal damage

CO(2) lasers can be operated at high laser pulse repetition rates for the rapid and precise removal of dental decay. Excessive heat accumulation and peripheral thermal damage is a concern when using high pulse repetition rates. Peripheral thermal damage can adversely impact the mechanical strength of the irradiated tissue, particularly for dentin, and reduce the adhesion characteristics of the modified surfaces. The interpulpal temperature rise was recorded using microthermocouples situated at the roof of the pulp chamber on teeth that were occlusally ablated using a rapidly-scanned CO(2) laser operating at 9.3 μm with a pulse duration of 10 to 15 μs and repetition rate of 300 Hz over a 2 min time course. The adhesion strength of laser treated enamel and dentin surfaces was measured for various laser scanning parameters with and without post-ablation acid etching using the single-plane shear test. The mechanical strength of laser-ablated dentin surfaces were determined via the four-point bend test and compared to control samples prepared with 320 grit wet sand paper to simulate conventional preparations. Thermocouple measurements indicated that the temperature remained below ambient temperature if water-cooling was used. There was no discoloration of either dentin or enamel laser treated surfaces, the surfaces were uniformly ablated, and there were no cracks visible. Four-point bend tests yielded mean mechanical strengths of 18.2 N (s.d. = 4.6) for ablated dentin and 18.1 N (s.d. = 2.7) for control (p > 0.05). Shear tests yielded mean bond strengths approaching 30 MPa for both enamel and dentin under certain irradiation conditions. These values were slightly lower than nonirradiated acid-etched control samples. Additional studies are needed to determine if the slightly lower bond strength than the acid-etched control samples is clinically significant. These measurements demonstrate that enamel and dentin surfaces can be rapidly ablated by CO(2) lasers with minimal peripheral thermal and mechanical damage and without excessive heat accumulation.