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Relationship between bond strengths and nanoleakage: evaluation of a new assessment method.

PURPOSE: To test if there was a correlation between resin-dentin bond strengths and nanoleakage of total etch and self-etching primer bonding systems. MATERIALS AND METHODS: Ten extracted third molars were ground flat with 600 grit SIC paper under running water to expose middle dentin. Clearfil Liner Bond 2V or Single Bond was applied to the dentin surface according to the manufacturers' instructions. A crown was built-up with Clearfil AP-X resin-based composite, and the specimens stored in water for 24 hrs at 37 degrees C. The bonded assemblies were cut mesiodistally perpendicular to the interface into approximately 0.7 mm thick slabs, and trimmed for microtensile bond strength testing. Alternate slices from each tooth were either entirely double-coated with nail varnish leaving a 0.5 mm window around the interface, or left uncoated to be immersed in water for 13 hrs as the control. The varnished (experimental) slabs were immersed in 50% AgNO3 for 1 hr, and then immersed in a photo developing solution for 12 hrs. All specimens were subjected to microtensile bond test at a crosshead speed of 1 mm/min. After debonding, the specimens were embedded in epoxy resin and observed under a confocal laser scanning microscope for determination of lateral silver penetration within the interface. Silver penetration was further analyzed under the SEM. Data were analyzed with one- and two-way ANOVA, Fisher's PLSD test (P < 0.05), and regression analysis. RESULTS: The bond strengths of Clearfil Liner Bond 2V and Single Bond were not significantly different (P > 0.05); however the bond strengths of the specimens that were soaked in 50% AgNO3 for 1 hr significantly increased (P < 0.01). No correlation was observed between bond strengths and nanoleakage.

Acid Etching, Dental↗

In vivo bonding mechanism of an experimental dual-cure enamel-dentin bonding system.

PURPOSE: To evaluate, in vivo, the formation of hybrid layer, resin tags and adhesive lateral branches, by an experimental dual-curing "one-bottle" enamel-dentin bonding system. MATERIALS AND METHODS: The new dentin adhesive (Excite DSC) was tested in five Class V restorations placed in vital, periodontally compromised teeth. The experimental bonding system was used in combination with a flowable composite. After 1 wk the teeth were extracted and processed for SEM evaluation. All the samples were split-fractured along their long axis. Half of the samples were used to evaluate hybrid layer formation and the other half to examine the morphology of resin tags. RESULTS: The experimental adhesive system showed a micromechanical bonding mechanism to conditioned dentin with formation of a hybrid layer, resin tags and adhesive lateral branches. SEM photomicrographs of the decalcified samples showed a high density of resin tags and uniform distribution along the cavity walls.

Composite Resins↗

SEM evaluation of the interaction between a three-step adhesive and dentin.

Interaction between resin tags and microtags of adhesive systems and dentinal collagen fibrils is a poorly understood aspect of adhesion. This study evaluated this interaction in 25 recently extracted human third molars. Each tooth was embedded in an epoxy resin and cross-sectioned to obtain two 1-mm-thick dentin disks. The outer dentin surfaces were polished with wet 600-grit sandpaper to create a uniform smear layer. After etching with 35% phosphoric acid for 15 seconds, the primer and adhesive of Scotchbond Multi-Purpose and the resin composite Z100 (3M Dental Products, St Paul, MN 55144, USA) were placed on the dentinal surfaces according to the manufacturer's instructions. The disks were left in distilled water at 37 degrees C for two weeks, then fractured perpendicular to the bonded surfaces in order to obtain two hemi-disks. The fractured surfaces were treated with 2N-chloridric acid and processed for scanning electron microscopy. Gold-coated specimens were examined with a JEOL 6100 scanning electron microscope. Results showed a hybrid layer with resin tags of approximately 100 microm in length and numerous and fine branching resin microtags. The tags and microtags created by this three-step adhesive system were observed in intimate contact with the collagen fibrils of dentin, even in deeper zones which were not affected by acid etching. It suggests that adhesion to dentin may include both micromechanical and chemical aspects.

Collagen↗

Relationship between nanoleakage and long-term durability of dentin bonds.

This study tested the hypothesis that long-term durability of resin bonds to dentin would directly relate to the nanoleakage of dentin bonding systems. Twenty extracted third molars were ground flat with #600 grit SIC paper under running water to expose middle dentin. One-Step or Single Bond was applied to the dentin surface according to the manufacturer's instruction. A crown was built-up with Clearfil AP-X resin composite and the specimens were stored in water for 24 hours at 37 degrees C. The bonded assemblies were cut mesio-distally perpendicular to the interface in approximately 0.7 mm thick slabs and trimmed for microtensile bond strength testing. All slabs were immersed in individual bottles containing 37 degrees C water that was changed daily. Specimens were randomly assigned to four groups (one day, three, six and nine months), and at the specified time period, the specimens to be tested were randomly divided into two subgroups for testing: 50% AgNO3 and the control. In the 50% AgNO3 subgroup, the slabs were coated with fingernail varnish except for approximately 0.5 mm around the bonded interface and immersed for one hour in 50% AgNO3, followed by exposure in a photo developing solution for 12 hours just prior to debonding. The specimens in the control subgroup were soaked in water until they were debonded. Then, all specimens were subjected to microtensile bond testing. Micrographs of the fractured surfaces of the debonded specimens in the AgNO3 subgroup were taken using light microscopy. They were then subjected to image analysis by NIH Image PC (Scion, Fredrick, MD, USA), and the area of silver penetration was quantitated. The fractured surface was further analyzed under the SEM. Bond strength data and the silver penetration areas were subjected to two and three-way ANOVA and Fisher's PLSD test at the 95% level of confidence. Regression analysis was used to test the relationship between bond strengths and the silver penetra tion area at each time period. The tensile bond strength of both materials gradually decreased over time. Specimens bonded with One-Step showed less silver nanoleakage at one day compared to three, six and nine months (p<0.05), but there were no significant differences between the nanoleakage measured at three, six and nine months. In contrast, for specimens bonded with Single Bond, there were no statistically significant differences in the silver nanoleakage among the four time periods tested (p>0.05). No correlation was observed between bond strength and nanoleakage for either bonding system. Nanoleakage occurred in both adhesive systems, and bond strengths gradually decreased over time. However, there was no correlation between bond strength and nanoleakage for either adhesive system in this study.

Analysis of Variance↗

Microtensile bond strength and confocal microscopy of dental adhesives bonded to root canal dentin.

PURPOSE: To evaluate the bond strength of two dentin-bonding systems to root canal dentin. MATERIALS AND METHODS: Six central incisors, extracted for periodontal reasons, were endodontically treated, no obturation of the root canal space was performed. The teeth were cut parallel to their long axis. One half of each tooth was randomly assigned to one of two experimental groups. The teeth of the first group were treated with All-Bond 2 dental adhesive and those of the second group with Panavia F. The root canal dentin was conditioned as suggested by the manufacturers and, after the application of the dental adhesives, a layer of resin-based composite was polymerized over the adhesive layer. After the composite had completely set, the sections were prepared for microtensile test and kept in a wet environment at a relative humidity of 90 +/- 2% measured with a digital relative humidity meter and at a temperature of 22 degrees C for 24 hrs. The specimens were sectioned perpendicularly to the bonded interface, into slabs 1.5 mm thick (10 sections for each experimental group). The slabs were then trimmed by super fine diamond burs for the microtensile bond test with the narrowest region located at the respective bonded interface. The thickness of the slab was then exactly established by three measurements performed in three points of each slab by a digital micrometer. The specimens were then subjected to a tensile force at a crosshead speed of 0.2 mm/min. The test was observed using a confocal microscope and the failure modes were noted. The load at failure was registered and the bonded area was measured using a confocal microscope at a magnification of x25 in conjunction with an image-processing program. The failure data were analyzed using the Wilcoxon-Gehan test with exact non-parametric inference. RESULTS: The mean value at failure was the same for the two experimental groups (17.1 MPa). There was no statistically significant difference between Panavia F and All-Bond 2 (P> 0.8671). Most of the specimens showed a debonding of the adhesive from the hybrid layer. The results showed that the bond strength of the two bonding systems tested to the dentin of the root canal are slightly lower than to those obtained with the latest adhesive systems, in the coronal dentin.

Composite Resins↗

Resin-tooth adhesive interfaces after long-term function.

PURPOSE: To characterize with scanning electron microscopy (SEM), the morphology of adhesive interfaces that had been functioning in an oral cavity for several years. MATERIALS AND METHODS: Cavities were prepared in vivo in caries-affected primary molars under local anesthesia. After removal of the entire carious lesion, the cavity was restored with a dentin adhesive system (Scotchbond Multi-Purpose). After several yrs, as the successor permanent teeth erupted, the resin-filled teeth were extracted. Then, the extracted resin-restored primary molars were cross-sectioned perpendicular to the adhesive interface using a low speed diamond saw and then polished for SEM examination. RESULTS: Morphological changes, such as digestion of the collagen fibrils and deterioration of the bonding resin and hybrid layer, were observed at the interface of the oral environment specimens. The results of this study demonstrated that degradation of resin-dentin bond structures appeared to occur in the human oral environment over time.

Child↗

Nanoleakage at the composite-dentin interface: a review.

The term "nanoleakage" was introduced to describe a specific type of leakage within the dentin margins of restorations. Nanoleakage appears as a consequence of the acid etching procedure allowing the penetration of oral and pulpal liquids such as acids into porosities within or adjacent to the hybrid layer. Nanoleakage is independent from microleakage. The amount of penetration depends on the type of bonding agent and on different parameters of the application technique (e.g. etching time, dentin moisture). Nanoleakage is much less extensive than microleakage and has probably no short-term clinical relevance. The long-term stability of the adhesive bond between dentin and restorative material, however, might be adversely affected. Nevertheless, based on the knowledge to date, acid etching prior to dentin bonding should be performed.

Acid Etching, Dental↗

Dentin bonding--questions for the new millennium.

PURPOSE: The objective of this review article is to summarize the most recent concepts in dentin bonding and, simultaneously, challenge some convictions that have not been backed up by sound, convincing research. After the introduction of the enamel acid-etch technique by Dr. Buonocore in 1955, the increasing demand for restorative and non-restorative esthetic treatments, as well as the refinement in the utilization of fluoride-containing products, have totally transformed the practice of operative dentistry. While bonding to enamel is a reliable technique, bonding to dentin represents a greater challenge: dentin is an intrinsically wet organic tissue penetrated by a tubular labyrinth containing the odontoblastic process, which communicates with the pulp. The manufacturers of new adhesive systems recommend the application of their adhesive materials on moist dentin. The main reason is that the spatial alteration that occurs upon drying demineralized dentin may prevent the monomers from penetrating the labyrinth of nano-channels formed by dissolution of hydroxyapatite crystals between collagen fibrils. Several of the current concepts in dentin bonding have been built from the observation of clinical studies, which measure retention rates, and from laboratory bond strength studies, which measure the force needed to debond a composite post from a flat dentin area. Although their utility is doubtful as far as clinical performance is concerned, bond strength studies are still necessary in order to compare similar parameters among materials. However, both clinical and laboratory studies lack information on the dynamic behavior of the substrate in a vital environment. For example, the changes induced by adhesive systems in the resin-infiltrated demineralized dentin have not been fully characterized. Also, the role of collagenous and non-collagenous proteins in dentin bonding has been generally overlooked.

Acid Etching, Dental↗

Distribution of nanofillers from a simplified-step adhesive in acid-conditioned dentin.

PURPOSE: This in vitro study examined the interfacial ultrastructure of a nanofilled, simplified-step adhesive (Prime & Bond NT, Dentsply), to determine the distribution of nanofillers within the collagen network of the hybrid layer. MATERIALS AND METHODS: Twenty-four dentin discs were divided into two groups and bonded using two recommended conditioning techniques: Group I, NRC (Non-Rinse Conditioner), and Group II, Conditioner 36 (colloidal silica thickened 36% phosphoric acid). Following conditioning, a single coat of adhesive was applied and light-cured. Dentin discs were then bonded to form disc-pairs and processed for TEM examination. Demineralized, ultrathin sections were examined stained or unstained. Non-demineralized sections were used for STEM/EDX analysis of elemental distribution across the resin-dentin interface. In addition, four dentin discs were bonded with a generic adhesive (HEMA/TBBO) for TEM examination of stained collagen and proteoglycans. RESULTS: In unstained sections of both groups, nanofillers from the adhesive layer were congested around patent tubular orifices, but were not found within the interfibrillar spaces of the hybrid layer. EDX analysis of silicon (Si) showed predominant distribution within the adhesive layer and tubular orifices. Phosphorus (P) was present within the hybrid layer and adhesive layer in Group II. CONCLUSION: It is hypothesized that a) aggregation of the nanofillers within the adhesive resulted in filler clusters that are too large to infiltrate the interfibrillar spaces of the hybrid layer; and b) retention of ground substance within the demineralized intertubular collagen matrix may also have prevented the infiltration of the nanofillers.

Acid Etching, Dental↗

Variable polymerisation shrinkage and the interfacial micropermeability of a dentin bonding system.

PURPOSE: Adhesive bonds are subjected to competing stresses whilst a restoration is setting. This study aimed to determine the effect of these stresses on a chemically- and light-activated dentin adhesive (Scotch Bond MultiPurpose Plus: SBMP+) by assessing the morphology and micropermeability of the interfacial region. MATERIALS AND METHODS: Restorative materials and techniques were selected to impart differing setting stresses to the adhesive interface. An amalgam (Dispersalloy), a light-activated composite (Z100) with a high- or low-intensity curing light, and chemically-activated composite (Adaptic) were placed either in bulk (4 mm thickness) or in one thin layer (2 mm) in occlusal cavities in 55 freshly extracted third molars. In addition, thin composite restorations were placed on 15 horizontally sectioned teeth using a glass slide as a rigid clear matrix. The pulp chambers of all samples were filled with rhodamine B dye solution for 4 hours. Samples were longitudinally sectioned and the interfacial dye leakage measured using a confocal optical microscope. Data were analysed using the Kolmogorov-Smirnov test. RESULTS: In occlusal cavities, Z100 had significantly more leakage than the amalgam and Adaptic. There was no significant difference in micropermeability between large and small increments, or curing light intensity for Z100, but when placed in bulk, there was evidence of incomplete composite polymerisation near the cavity floor, especially with the low intensity curing light. Cohesive failure of the deep resin composite and gap formation were a frequent finding with the high-intensity light curing. The least leakage for Z100 was achieved with a thin layer on flat dentin. In contrast, the chemically-activated composite performed well in bulk when the surface of the restoration was freely exposed, but badly when constrained by the glass matrix. CONCLUSION: Restoration setting stress is critical in the microscopic integrity of the adhesive bond to dentin.

Bisphenol A-Glycidyl Methacrylate↗

Interfacial micromorphology and tensile bond strength of dentin bonding systems after NaOCl treatment.

PURPOSE: The objective of this study was to test the hypothesis that NaOCl treatment of acid-etched dentin would not lower the tensile bond strength of adhesive resins, but would eliminate the hybrid layer. MATERIALS AND METHODS: One hundred twenty teeth and three different bonding agents were used for SEM- and CLSM-visualization of the dentin-composite interface and for bond strength measurements. After etching with phosphoric acid, 75 dentin samples were pretreated with 10% NaOCl. The other 75 samples were etched only with phosphoric acid and were kept as controls. Composite was bonded to the pretreated surfaces with a bonding resin. RESULTS: NaOCl-treated samples: hybrid layers were not visible, but resin tags and resin penetration through lateral branches of tubules were prominent. Layers of unfilled resin were not apparent for Gluma CPS and Prime & Bond 2.1. Hypochlorite treatment of acid-etched dentin resulted in reduced bond strengths for specimens bonded with Syntac and Gluma CPS, but such treatment increased bond strength for Prime & Bond 2.1 bonded specimens. CONCLUSION: The removal of the collagen layer with NaOCl can enhance or decrease bond strengths, depending on the bonding agent used.

Composite Resins↗

Hybridization effectiveness of a two-step versus a three-step smear layer removing adhesive system examined correlatively by TEM and AFM.

PURPOSE: The objectives of this study were (1) to compare the hybridization effectiveness of two adhesive systems that are applied in respectively three and two steps, and (2) to determine the best resin-dentin interface preparation technique for atomic force microscopy (AFM). MATERIALS AND METHODS: The resin-dentin interface produced by the three-step OptiBond Dual-Cure (Kerr) and its simplified two-step successor OptiBond Solo (Kerr) was ultramorphologically examined using transmission electron microscopy (TEM) and AFM. Four different methods were used to prepare interface specimens for AFM: (1) polishing to a 0.1-micron finish with a silicon oxide suspension, (2) polishing to a 0.05-micron finish with an aluminum oxide suspension, (3) argon-ion etching, and (4) sectioning with a diamond knife. RESULTS: Both TEM and AFM demonstrated that some collapse of the exposed collagen fibril network, due to gentle postconditioning air-drying of the dentin surface, may not have been totally recovered through hybridization by the two-step adhesive formulation as opposed to the three-step precursor. From the four interface preparation methods, only diamond-knife sectioning revealed sufficient ultramorphologic detail and high resolution that can capitalize on the high resolution offered by AFM. CONCLUSION: First, the findings suggest that simplifying the application procedure of adhesives by combining the primer and adhesive resin into a single application step may reduce hybridization effectiveness. Future research should confirm this effect for other two- versus three-step adhesive systems. Second, diamond-knife sectioning should be used for future topographic imaging and physicomechanical testing of resin-dentin interfaces by AFM.

Bisphenol A-Glycidyl Methacrylate↗

Effect of collagen removal on microleakage of resin composite restorations.

This study evaluated the effects of collagen removal on the microleakage of two single-bottle adhesive systems. Forty human third molars were selected and each received two root preparations. The roots were randomly assigned for restoration using Prime & Bond 2.1 (Dentsply Ltda, Petrópolis, RJ 90915, Brazil) or Single Bond (3M Dental Products, St Paul, MN 55144, USA). One root in each tooth was treated with 36% H3PO4 for 15 seconds and the other received an additional treatment with 10% NaOCl for 60 seconds to remove the collagen layer before adhesive was applied. All preparations were restored with Z100 restorative resin (3M Dental Products). The specimens were submitted to 5,000 thermal cycles (5-55 degrees C) and stored in 37 degrees C distilled water for one year. The specimens were then coated with a varnish except for 1 mm of tooth structure surrounding the restoration and immersed in 2% buffered methylene blue for four hours. After rinsing, the restorations were sectioned and two independent observers scored the microleakage at the interface between the restorative material and the tooth using an optical microscope at x45 magnification. The scores were submitted to Fisher's Exact Test and the results showed that collagen removal significantly reduced microleakage for Prime & Bond 2.1 and had no effect on microleakage for Single Bond.

Acetone↗

Scanning electron microscopy evaluation of the interface of three adhesive systems.

The objective of this research was to investigate the resin-dentin interface of three adhesive systems, Scotchbond Multi-Purpose, Optibond and Denthesive Bond II by scanning electron microscopy. The adhesives and their respective composite resins were applied inside the cervical root canal of human incisors and canines according to manufacturer recommendations. The teeth were embedded in acrylic resin and sliced transversally to the root canal and perpendicularly to the resin-dentin interface. The adhesive systems Scotchbond Multi-Purpose and Optibond had a homogenous hybrid layer and similar characteristics, involving resin penetration of peritubular and intertubular dentin matrix. Morphological differences of resin tags were seen; Scotchbond Multi-Purpose had more and longer tags than Optibond. Denthesive Bond II did not have the same consistency of bonding. Tubular orifices were not opened and the smear layer was not removed. This was due to the absence of previous acid conditioning of dentin that damages hybrid layer formation. Analysis of the hybrid layer revealed different patterns, suggesting that the attachment was influenced by many factors and a standardization of dentinal substrate was impossible.

Adhesives↗

Fractographical analysis of resin-dentin bonds.

PURPOSE: To characterize resin-dentin bond structures of three adhesive resin systems using fractographic analysis to measure the area of failure at the fractured surface. MATERIALS AND METHODS: Flat dentin surfaces were ground perpendicular to the long axis of the tooth. The prepared dentin surfaces were treated by one of three adhesive resin systems (Mac Bond II, One-Step, and Single Bond). The samples were sectioned perpendicular to the adhesive interface to produce a square bar-shaped specimen (adhesive area: 0.9 mm2) using a diamond saw. A micro-tensile test was then conducted at a crosshead speed of 1.0 mm/min. The mean tensile bond strengths were statistically compared using one-way ANOVA and Fisher's PLSD test (P< 0.05). The fractured surfaces of all specimens were examined using SEM and the area of failure was measured using an image analyzer on SEM microphotographs. RESULTS: No significant differences in tensile bond strength were observed between Single Bond (62.1+/-18.2 MPa) and One-Step (53.8+/-13.1 MPa) (P > 0.05). However, the bond strength of Mac Bond II (36.5+/-13.7 MPa) was significantly lower than that of One-Step or Single Bond (P< 0.05). At the fractured surface, except for the cohesive failure of the bonding resin and resin-based composite, different failure patterns were observed for each resin system as follows: the failure of the hybrid layer and demineralized dentin was observed in the two wet bonding systems (One-Step and Single Bond) and of the hybrid layer but not the demineralized dentin in the self-etching primer system (Mac Bond II). The results demonstrated that the integrity of the hybrid layer depends on the adhesive system.

Analysis of Variance↗

Influence of a simulated oral environment on dentin bond strength of two adhesive systems.

PURPOSE: To evaluate in vitro the influence of different clinical conditions (temperature, relative humidity) on dentin bond strength. MATERIALS AND METHODS: Two different bonding systems were studied, ScotchBond Multi-Purpose Plus (SBMP) and Clearfil SE Bond (SE Bond). In the first part of the study, the different environmental conditions were: ambient conditions, i.e. 20 degrees C/30% relative humidity (RH), 30 degrees C/50% RH, 30 degrees C/65% RH, 33 degrees C/80% RH and 35 degrees C/95% RH. In the second part, the different interfaces (dentin/primer, primer/adhesive and adhesive/composite for SBMP and primer/adhesive, adhesive/composite for SE Bond) were also studied in order to explain the results obtained in the first part of the study. After the bonding procedure, a composite cylinder (Z100) was bonded to the surface using a Teflon mold (diameter: 3 mm/height: 5 mm). The different specimens were tested in a shear bond mode after a 24-hour storage in distilled water at 37 degrees C. RESULTS: For SBMP, the shear bond strengths decreased when temperature/RH increased. The average values were very low when the 35 degrees C/95% RH conditions were simulated. A study of the interfaces showed that the primer/adhesive interface was the most sensitive to the environmental conditions simulated. For SE Bond, a decrease occurred but only at the highest temperature/humidity conditions. The interface study did not provide an explanation of the results obtained in the first part of the study.

Analysis of Variance↗

Micromorphological study of resin-dentin interface of non-carious cervical lesions.

This study examined the interfaces between two dentin adhesives, namely, One Coat Bond, Clearfil SE Bond and a resin-modified glass ionomer cement (Fuji II LC) and the dentin of non-carious cervical lesions (NCCLs) with FE-SEM, and compared them with the interfaces produced with "normal" dentin. Fifteen human premolars each with a buccal NCCL were used. Cervical cavities were prepared on the lingual surface of the same teeth for the normal (control) dentin. All lesions and prepared cavities were cleaned with a slurry of pumice and water. The teeth were randomly divided among the three products that were applied according to the manufacturers' instructions. For the resin-bonded specimens, the cavities were restored with resin composite. All specimens were stored in 37 degrees C tap water. Resin-bonded specimens were observed using FE-SEM after treatment with 10% phosphoric acid, and 10% phosphoric acid and 5% sodium hypochlorite (NaOCl). The resin-modified glass ionomer cement (RM-GIC) specimens were observed after 10% phosphoric acid and 5% NaOCl treatment. The hybrid layer could be observed for the two adhesive systems in all specimens, but the thickness varied depending on the bonding system used and the dentin substrate. The results suggested that the hybrid layer produced in normal dentin was slightly thicker than that of NCCLs. Further, the hybrid layer thickness decreased in all specimens after NaOCl treatment.

Bicuspid↗

Dentine bonding agents--a review of adhesion to dentine.

Although constant innovation has improved the performance of dentine adhesives, the true mechanism of resin adhesion to dentine is still not clear and the optimal dentinal surface pretreatment has yet to be determined for adhesive integrity of resin to dentine. The integrity of the collagen fibrils left exposed upon acid etching seem to play a major role in the mechanism of adhesion and intermingling of the adhesive monomers with the filigree of collagen fibers or hybrid layer should be considered the paramount dentine bonding mechanism. Definite trends are emerging but more research is necessary before general conclusions can be made about the functions of different bonding agents. The all-in-one self-etching/self-primer bottle systems are relatively new to the market and need more research before they can be advocated as the agent of choice.

Acid Etching, Dental↗