Dentin bonding as a function of dentin structure

The traditional principles of operative dentistry have been challenged since Dr. Buonocore introduced the aid-etch technique in 1955. In spite of the numerous changes in clinical protocols and adhesive techniques, adhesion to dentin remains difficult. The importance of micromechanical bonding to dentin has been recognized over the last decade. Researchers now believe that dentin adhesion relies primarily on the penetration of adhesive monomers into the filigree of collagen fibers left exposed by acid etching. Two main strategies are currently in use for bonding to enamel and dentin: the self-etch technique and the total-etch technique. The efficiency of either bonding strategy depends very much on the dentin substrate used for bonding. Laboratory tests use ideal dentin from extracted teeth, which does not reflect the clinical reality. Clinical studies are the ultimate test for any dental adhesive material.     

Evaluation of the bonding mechanism of an adhesive material to primary teeth

PURPOSE: The aim of this study was to evaluate with scanning electron microscopy (SEM) the bonding mechanism of the one-bottle adhesive Prime&Bond NT (Dentsply, PBNT) to enamel and dentin of deciduous teeth, following different methods of substrate treatment. METHODS: Eighteen extracted posterior deciduous teeth were randomly divided into 6 groups (N=3). The experimental groups differed for substrate and method of substrate conditioning prior to bonding with PBNT. Group 1: 36% phosphoric acid (PA)/PBNT on dentin; group 2: PA/PBNT on enamel; group 3: non-rinsing conditioner (NRC) (Dentsply)/PBNT on dentin; group 4: NRC/PBNT on enamel; group 5: PBNT on dentin without any previous conditioning; group 6: PBNT on enamel without any previous conditioning. On all the specimens, following the application of the adhesive solution, Dyract AP was layered on top and light-cured. The bonded specimens were processed for SEM observations. RESULTS: When used in combination with 36% phosphoric acid, PBNT was able to form a hybrid layer with resin tags on both enamel and dentin. Following conditioning with NRC, a thinner hybrid layer with shorter resin tags was developed on dentin; on enamel an etching pattern was still detectable. When only PBNT was applied without any previous conditioning, on dentin neither hybrid layer nor resin tags were visible; no sign of micromechanical bonding could be seen on the untreated enamel. CONCLUSIONS: The bonding mechanism of the one-bottle adhesive Prime&Bond NT on enamel and dentin of deciduous teeth is effective only following substrate conditioning with 36% phosphoric acid or NRC.     

Adhesive dentistry: the development of immediate dentin sealing/selective etching bonding technique

A major objective of dental research over the past 60 years has been a search for the "dream-team" of dental adhesives. In fact, a recent Medline search produced more than 6,500 papers on dentin bonding and its techniques. Adhesive systems are designed to retain direct and indirect restorations, minimize leakage at the margin, and be simple to place while producing consistent results. The development of materials and techniques has an interesting history; some have recirculated from the past and are being used in some form today. Buonocore used the etchant phosphoric acid at the beginning of the adhesive revolution. Though not accepted for many years it eventually became the "gold standard" for etching enamel. Technique sensitivity moved it out of favor and, through the development of self-etching acidic primers, was eliminated from some adhesive systems. Although these primers may have successfully addressed postoperative sensitivity, adhesion was compromised. The bond strength of these systems has now been improved with the incorporation of phosphoric acid-etch to condition enamel prior to using the adhesive system. This article will trace the history of adhesive techniques and materials and how it has led to the creation of a new technique that combines two bonding methods.     

Effect of ferric chloride/citric acid/phosphoric acid conditioner on adhesion of 4-META/MMA-TBB resin to the tooth

The aim of this study was to examine the effects of ferric chloride/citric acid/phosphoric acid conditioners on the surface morphology of enamel and dentin and on the adhesion of 4-META/MMA-TBB resin to conditioned tooth surfaces. Seven conditioners, including phosphoric acid and its mixture with citric acid and ferric chloride, were prepared and used for treating bovine teeth before bonding with the resin. The effects of the conditioners on the surface morphology and adhesion were examined by scanning electron microscopy and by atomic force microscopy and by tensile bond strength tests, respectively. The maximum bond strengths to tooth surfaces were obtained by using 3% ferric chloride/5% citric acid/10% phosphoric acid conditioner. Thus, enamel and dentin can be treated simultaneously with this conditioner before bonding with the 4-META/MMA-TBB resin system.     

Evaluation of the F2000 bonding procedure: a high resolution SEM study.

OBJECTIVES: The aim of this study was to define the morphological bonding of the F2000 Restorative System (3M Dental Product) to enamel and dentin. For this purpose, high resolution scanning electron microscope (SEM) in conjunction with a tensile bond strength analysis was used to correlate the morphological findings to the bonding potential. Scotchbond 1 (SB1) adhesive system was utilized as a control. MATERIALS AND METHODS: Teeth were prepared in vivo and prepared as: (1) F2000 PA for 15s, (2) F2000 PA for 30s, (3) 35% phosphoric acid for 15s and SB1 and (4) 35% phosphoric acid for 30s and SB1. All teeth were then restored with the F2000 compomer restorative material, extracted, sectioned and analyzed by means of a field emission in-lens SEM (FEISEM). The conditioning/etching patterns of the two adhesive systems were also evaluated in vitro on dentin disks in order to show high resolution details of every single step of the bonding procedure. RESULTS: FEISEM images showed a repetitive pattern of the enamel crystals with several microporosities after the 30s application of F2000 PA; moreover a good adaptation of the adhesive resin on the conditioned enamel was observable. FEISEM analysis of the dentin surface revealed no evidence of a smear layer after the application of F2000 PA for 30s. Residual smear plugs were partially obliterating the tubule orifices when F2000 PA was used, while they were completely absent after etching with 35% phosphoric acid. The total etching technique revealed open tubules and resin tags formation after the application of SB1. CONCLUSIONS: The one step etching/priming/bonding procedure of the F2000 PA showed favorable results at ultra-structural level when applied on both the enamel and the dentin surface for 30s (as per manufacturers' instructions), but the bond strength analysis showed higher values of bonding of the F2000 compomer when the SB1 adhesive agent (after etching with 35% phosphoric acid) was used (7.7+/-2.2 vs 19.0+/-4.4MPa).     

Shear bond strength of current adhesive systems to enamel, dentin and dentin-enamel junction region

This study investigated the bonding of current resin adhesives to the region approximating the dentin-enamel junction (DEJ), where the etch pattern to enamel or dentin may be different. Three kinds of tooth substrates were chosen for testing: enamel, dentin and the DEJ region. A self-etching primer system (Clearfil SE Bond) and two total-etch wet bonding systems (Single Bond and One-Step) were used. Each tooth region was bonded with one of the adhesive systems, and a resin composite and was subjected to a micro-shear bond test. In addition, morphological observations were performed on debonded specimens and etched surfaces using confocal laser scanning microscopy (CLSM). CLSM observations showed that the DEJ region was etched more deeply by phosphoric acid gel than enamel or dentin, suggesting that the action of acid etch seemed to be more intense on the DEJ. However, no statistically significant differences of shear bond strength values were observed between the DEJ region and enamel or dentin, or the adhesive systems used (p>0.05). Bonding to the DEJ is potentially as good as that to enamel or dentin.     

In vitro bracket bond strength to acid-etched or air-abraded enamel.

PURPOSE: This study evaluated, in vitro, the capacity of a dentin bonding agent to improve the bond strength of orthodontic brackets using air abrasion enamel preparation. METHODS: Each of the enamel surfaces received a different treatment prior to bonding procedures. Group 1 received acid-etched with 38% phosphoric acid for 30 seconds. Group 2 received acid-etched with 38% phosphoric acid for 30 seconds, dentin bonding agent (Scotchbond MultiPurpose) applied after rinse completed. Group 3 received abrasion-etched (particle size 50 microns, 120 psi). Group 4 received abrasion-etched, dentin bonding agent applied after etching completed. Unfilled adhesive resin (Ormco light cured sealant) was applied followed by a premolar bracket (Ormco meshed mini-twin) with adhesive (Ormco light cured adhesive) placed on the back. Shear bond strengths were measured using an INSTRON machine and the site of bond failure was determined under 3X magnification. RESULTS: The shear bond strength obtained with a traditional acid-etch, in vitro, was not improved significantly by the use of a dentin bonding agent. Air abraded surfaces showed very low bond strengths with all treatments. CONCLUSIONS: Tested in vitro, air-abraded surfaces provide clinically unacceptable bond strength when compared to acid-etched enamel surfaces.     

Bond strengths of nonrinsing adhesives.

OBJECTIVE: The purpose of this study was to determine enamel and dentin bond strengths of a nonrinsing "all-in-one" adhesive and of a nonrinsing conditioner combined with a 1-bottle adhesive. METHOD AND MATERIALS: Specimens were obtained from 240 bovine teeth ground to expose enamel or dentin surfaces. Ten enamel and 10 dentin specimens were randomly assigned to each of 12 different combinations of adhesive system (Prompt L-Pop; no etch + Prime & Bond NT; NRC + Prime & Bond NT; 36% phosphoric acid + Prime & Bond NT; no etch + Prime & Bond 2.1; 36% phosphoric acid + Prime & Bond 2.1) and restorative material (resin composite; polyacid-modified resin composite ["compomer"]). After the application of the adhesive system, a No. 5 gelatin capsule filled with the restorative material was seated against the enamel or dentin surface. After 24 hours in distilled water at 37 degrees C, the specimens were thermocycled and the shear bond strengths were measured. RESULTS: For resin composite, etching with phosphoric acid resulted in the highest bond strengths to enamel. For compomer, the highest enamel bond strengths were achieved with both phosphoric acid and Prompt L-Pop. Treating dentin with Prime & Bond NT without etching provided the highest mean bond strength for composite. For compomer, treating dentin with Prime & Bond NT resulted in the highest mean bond strengths, regardless of the conditioner. CONCLUSION: Compomer and resin composite exhibited statistically similar bond strengths. Bond strengths to dentin were significantly lower than those to enamel.     

Adhesive restorative materials: a review

'Adhesive' restorative dentistry originated with the work of Buonocore in 1955 in bonding resin to etched enamel. Since then, adhesive materials and techniques have developed at a rapid rate. The first chemically adhesive material (zinc polycarboxylate cement) was marketed in the late 1960s, and glass-ionomer cements and dentine bonding agents have since become available. This review focuses on the latter two products. Glass-ionomer cements have a particular role in adhesive dentistry because of their reliable chemical adhesion to enamel and dentine, and because of their apparent ability to promote the remineralization of 'affected' dentine. Dentine bonding agents have undergone marked changes in presentation over the last 15 years, but all have an essentially similar bonding system, that of hybrid layer formation. However, the most recent systems have limited clinical data supporting their use.     

Effects of the XR bonding system on microleakage

Bonding of composite resins to dentin is generally less effective and less predictable than bonding to enamel. Several new dentin bonding agents have been developed to improve adhesion. One of these products, the XR Bonding System, includes a glass ionomer liner and a resin dentin adhesive. Our study found that the resin dentin adhesive (primer and bonding agent) did not reduce microleakage effectively. However, when used in combination with the glass ionomer liner, the resin bonding system allowed very minimal microleakage.     

Adhesion to dentin by means of Gluma resin

Abstract – In its present version, the Gluma system for bonding restorative resin to dentin involves the application of an enamel bonding agent prior to the composite resin. Conceivably, pretreating the dentin with solutions of amino acids, and incorporating camphorquinone and selected methacrylic monomers into the Gluma adhesive would nullify the need for the enamel bonding agent. A bond strength to dentin of 13.4 MPa was obtained in the control experiment. Using a solution of pyruvic acid and glycine as pretreatment, and an optimized adhesive mixture containing glutaraldehyde, HEMA, BIS-GMA, camphorquinone, and water, bond strengths to dentin of 14.5 MPa and to enamel of 23.3 MPa were obtained. Thus, the new Gluma bonding system gave acceptable bond strengths without the prior application of enamel bonding agents.     

Adhesion to dentin by means of Gluma resin

In its present version, the Gluma system for bonding restorative resin to dentin involves the application of an enamel bonding agent prior to the composite resin. Conceivably, pretreating the dentin with solutions of amino acids, and incorporating camphorquinone and selected methacrylic monomers into the Gluma adhesive would nullify the need for the enamel bonding agent. A bond strength to dentin of 13.4 MPa was obtained in the control experiment. Using a solution of pyruvic acid and glycine as pretreatment, and an optimized adhesive mixture containing glutaraldehyde, HEMA, BIS-GMA, camphorquinone, and water, bond strengths to dentin of 14.5 MPa and to enamel of 23.3 MPa were obtained. Thus, the new Gluma bonding system gave acceptable bond strengths without the prior application of enamel bonding agents.     

Critical appraisal. Dentin bonding: matrix metalloproteinases and chlorhexidine

Contemporary resin-dentin bonding is initiated by systems that use phosphoric acid or acidic resin monomers to remove mineral, exposing the superficial dentin collagen matrix. Collagen-associated proteins, including enzymes known as matrix metalloproteinases (MMPs), also are exposed. The collagen matrix is subsequently infiltrated with resins that are polymerized to establish an adhesive attachment to the dentin. Exposed collagen matrix that is not infiltrated with the adhesive can be degraded by associated MMPs, which might result in deterioration of the adhesive-dentin bond over time. Chlorhexidine (CHX) is able to inhibit MMPs by binding calcium and zinc ions necessary for proteolytic activity. This Critical Appraisal presents salient publications on research that evaluate CHX and its ability to limit MMP degradation of dentin bonds created by etch-and-rinse and self-etch adhesive systems.     

Effect of removal of surface collagen fibrils on resin-dentin bonding.

OBJECTIVES: The aim of this study was to evaluate the effects of NaOCl at removing the demineralized layer by examining the morphology of the hybrid layer and measuring shear bond strengths after different dentin treatments. METHODS: Dentin disks were treated with: (1) 35% phosphoric acid (PA) 20 s; (2) PA treatment followed by 1.5% NaOCl, 2 min; (3) PA treatment, followed by a 10% NaOCl immersion for 120 h. SEM was used to analyze the morphology of dentin and its interface with dentin bonding agents (DBAs), while shear bond strength tests were used to measure adhesion. All specimens were then fractured into two halves: One half was inspected under SEM; the other half was sequentially placed in 10% PA followed by 12.5% NaOCl for 70 h, to remove all dentin from the resin replica of the original bonded interface. RESULTS: SEM observations showed that collagen fibrils were completely removed from the acid-etched surface by NaOCl treatment. The diameter and the size of dentinal tubules and the number of lateral branches of the tubules were increased following NaOCl treatment. NaOCl applied on dentin smear layers did not significantly modify their SEM morphology. Resin tags were larger in diameter after phosphoric acid/NaOCl treatment than after only phosphoric acid treatment. Resin-infiltrated dentin-layers were only observed after the single phosphoric acid (i.e. conventional etching) procedure, and were not observed after combined phosphoric acid/NaOCl treatment. Etched/NaOCl samples showed a lower bond strength using Scotchbond MP and 3M Single Bond, but were higher in Optibond FL and unmodified in Prime & Bond 2.0 groups when compared with acid-etched controls. Treatment of etched dentin with NaOCl for 120 h produced an unusual type of resin infiltration of mineralized dentin that could be called a "reverse hybrid layer" which may explain the mechanism of resin bonding to NaOCl treated dentin. SIGNIFICANCE: The use of acidic conditioners for exposure of the collagen matrix exposes a soft delicate mesh that can collapse, thereby interfering with resin infiltration. If acid-etching is followed by NaOCl treatment, high bond strengths can be achieved via "reverse hybrid layer" formation, a proposed new mechanism of micromechanical resin retention. This mechanism is not yet recommended for clinical use but demonstrates a new type of resin retention.     

Shear bond strength of new self-adhesive flowable composite resins

Recently, new self-adhesive flowable composite resin systems have been introduced to the market. These new composite resin systems reportedly bond to dentin and enamel without the application of an adhesive bonding agent. The purpose of this study was to evaluate the shear bond strength to enamel of two new self-adhesive flowable composites with and without the use of an etch-and-rinse bonding agent. The new self-adhesive flowable composites had significantly lower bond strengths to enamel compared to a traditional adhesively bonded flowable composite. Both self-adhesive flowable composites had a significant increase in bond strength to enamel with the use of a phosphoric acid-etch and adhesive bonding agent.     

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.     

A confocal microscopic evaluation of resin-dentin interface using adhesive systems with three different solvents bonded to dry and moist dentinan in vitro study.

OBJECTIVE: Total dehydration of acid-etched dentin is known to cause the collapse of collagen fiber, which leads to poor hybridization. Dentin-bonding systems with water as a solvent are found to rehydrate the collapsed collagen. Acetone-based adhesives are found to compete with moisture, and the acetone carries the resin deep into the dentin. The question arises whether to dry the dentin and use a water-based adhesive, or to keep the dentin moist and use an acetone- or alcohol-based adhesive. The aim of this study was to compare different bonding systems and techniques to assess which is most successful. A confocal microscope was used to evaluate the amount of hybrid layer formation and the depth of resin tag formation. METHOD AND MATERIALS: Superficial occlusal dentin specimens from 120 noncarious, freshly extracted human premolars were used for the study. The dentin was etched using 36% phosphoric acid for 15 seconds and then rinsed. The specimens were then randomly divided into 4 groups for different drying procedures: group I: air-dried for 30 seconds; group II: air-dried for 3 seconds; group Ill: blotted dry; group IV: overwet. The specimens were further subdivided into 3 groups to be tested with different bonding systems: subgroup A: acetone-based adhesive (Prime & Bond NT); subgroup B: water-based adhesive (Syntac Single Component); subgroup C: water- and ethanol-based adhesive (Single Bond). The resulting resin-dentin interfaces were then examined and categorized via confocal microscopy, and relative values were assigned to each specimen. RESULTS: Group IV (overwet) showed the lowest values, and the highest values were obtained in group III. The highest values were seen in group III, subgroup A (blotted dry, acetone-based bonding agent, Prime & Bond NT). CONCLUSION: Under these conditions, using these three bonding systems, maximum hybridization and resin tag formation was achieved using acetone-based adhesive on etched dentin kept moist by blot drying.     

Adhesion of light-cured composite resin to bleached and unbleached bovine dentin

Abstract Cylinders of small-particle light-cured composite resin were bonded to the superficial dentin layer of young bovine incisors that had previously been subjected to 4 different treatments: 1) immersed in 35% hydrogen peroxide for 60 min, then etched with 37% phosphoric acid gel for 60 s; 2) immersed in saline for 60 min, then etched with 37% phosphoric acid gel; 3) etched with 37% phosphoric acid gel for 60 s, then immersed in 35% hydrogen peroxide for 60 min; and 4) etched with 37% phosphoric acid gel, then immersed in saline for 60 min. Specimens were stored in water at 37°C for 1 and 7 d prior to tension and shear testing. A total of 128 teeth were tested: 8 teeth in each group, for each day and for each test. No measurable adhesion of resin to peroxide-treated dentin was observed and statistical analysis of the test results indicated that this represented a highly significant reduction in the bond strength as compared with values obtained when resin bonded to saline-treated dentin was tested. SEM examination of randomly selected fracture test specimens indicated that the bond failure was both cohesive and adhesive in nature, suggesting that peroxide treatment adversely affects the setting of bonding resin and its adhesion to a filled resin.     

Increases in dentin-bond strength if doubling application time of an acetone-containing one-step adhesive

This study investigated the microtensile bond strength (microTBS) of a one-step self-etching adhesive to human dentin and bovine enamel following different bonding treatments. Occlusal portions of human molars and labial surfaces of bovine incisors were ground flat to provide uniform dentin and enamel surfaces, respectively. Futurabond was used following five different protocols: 1) according to the manufacturer's directions, 2) acid etched with 36% phosphoric acid (H3PO4) for 15 seconds, 3) 10% sodium hypochlorite (NaOCl) treated for two minutes after H3PO4-etching, 4) doubling the application time of the adhesive and 5) doubling the number of adhesive coats. Composite build-ups (6 mm in height) were constructed incrementally with Arabesk resin composite. The specimens were stored in 100% humidity for 24 hours at 37 degrees C and sectioned into beams of 1.0 mm2 cross-sectional area. Each beam was tested in tension in an Instron machine at 0.5 mm/minute, and mean microTBS data (MPa) were analyzed by one-way ANOVA and post-hoc multiple comparisons tests (alpha = 0.05). Doubling the application time of Futurabond attained the highest microTBS to dentin; whereas, no differences among all bonding application parameters evaluated could be detected when the adhesive was applied to enamel.     

Extension of a one-step self-etch adhesive into a multi-step adhesive.

One-step self-etch adhesives are undoubtedly the most user-friendly adhesives, but have been associated with lower bonding effectiveness as compared to two-step and three-step adhesives. Conversion of a one-step self-etch system into a two-step self-etch adhesive by adding a bonding step, or into a three-step etch&rinse adhesive by adding a beforehand etching step and a bonding step might be tempting in order to improve bond strength. OBJECTIVES: The objective of this study was to investigate whether adding application steps influences the bond strength of a one-step self-etch adhesive. METHODS: In this study, the bonding effectiveness of two experimental one-step self-etch adhesives and three different commercial adhesives to enamel and dentin was determined using a micro-tensile bond-strength protocol. This procedure was repeated for the experimental adhesives transformed into two-step self-etch and three-step etch&rinse adhesives. In addition, their interaction with tooth tissue was investigated using TEM and Feg-SEM. RESULTS: Transforming a one-step into a two-step self-etch adhesive did improve the bond strength to enamel and dentin, though not significantly. By adding a preceding etching step, the bond strength to enamel was significantly improved, but that to dentin was decreased considerably. The latter must be attributed to hampered resin infiltration of the one-step self-etch adhesive within the relatively deeply exposed collagen fibril network. SIGNIFICANCE: Additional application of a hydrophobic bonding agent slightly improved bonding effectiveness. Adding a preceding etching step is beneficial for enamel but should be avoided for dentin as this will decrease bond strengths, and may even jeopardize the bonding durability.