Resin-dentin Interdiffusion Zone Research Articles

A scanning electron microscope-based comparative evaluation of resin tag formation at the resin dentin inter-diffusion zone

Aim of study was evaluate and compare the formation of the resin dentin interdiffusion zone (RDIZ) at the radicular dentin and resin interface after etching with phosphoric acid (PA) and glycolic acid (GA), using either light-cure and self-cured adhesives. Twenty extracted teeth were root canal treated. Post space preparation was done, and the samples were randomly divided into two main groups depending upon the etchant. Each group was further divided into two subgroups depending on the type of adhesive used. One group was etched with 37% PA (Prime® Dental Products PVT LTD, India) and the other with 35% GA (Glycolic 35 Peel, Rejsol, India). Etching was followed by the application of light-cured adhesive (3M ESPE Adper Single Bond, USA) or self-etch (3M ESPE Single Bond Universal, Germany). Fibre posts were then placed and after a coronal build-up, the teeth were sectioned longitudinally and observed under SEM. Statistical analysis: Data was analyzed by descriptive statistics as a percentage of resin tag density for all the groups. The Kruskall-Wallis test was applied for overall comparison and a Mann-Whitney U test for inter-group analysis. Resin tag density was found to be the highest in the coronal third followed by the middle third of radicular dentin and was the least in apical thirds for both groups. Resin tag density was similar for light cure and self-etch adhesives in the coronal, middle, and apical thirds of both groups. In conclusion this study concluded that GA could be thought of as a potential etchant for the radicular dentin.

High-resolution mechanical mapping of the adhesive–dentin interface: The effect of co-monomers in 10-methacryloyloxydecyl dihydrogen phosphate

The presence of 10-methacryloyloxydecyl dihydrogen phosphate (MDP) at the adhesive–dentin interface enables ionic binding to calcium salts, which results in rigid nano-layering within the submicron scale resin–dentin interdiffusion zone. MDP has been used with additional co-monomers, such as hydroxyethyl methacrylate (HEMA) and/or 4-methacryloyloxyethyl-trimellitic acid (4-MET), mainly to enhance the chemical bonding properties. However, the use of co-monomers may compromise the rigidity of the adhesive–dentin interface. In this study, we use high-resolution mechanical mapping across the interface to discern the in situ mechanical properties of each target region at the nanoscale. Visualization by modulus mapping demonstrated that HEMA increases the diffusion properties of MDP into dentin structures. However, the rigidity of the adhesive–dentin interface indicated by the storage modulus was markedly lower in MDP containing HEMA than in MDP containing 4-MET. Dynamic indentation testing revealed that the bonding layer was more deformable in the presence of HEMA. Moreover, the presence of MDP in the bonding layer might also increase the deformability because the polymerization linearity allows a large degree of viscoelasticity. These factors also diminish the rigidity of the adhesive–dentin interface. Within the limitations of this study, our findings demonstrated that 4-MET is a better co-monomer than HEMA in MDP-based dental adhesives. Modulus mapping and nanoindentation are introduced as new tests for the adhesive–dentin interface to address queries about the effectiveness of dental adhesives.

A zinc chloride-doped adhesive facilitates sealing at the dentin interface: A confocal laser microscopy study

The aim of this study was to ascertain the effect of Zn-doping of dental adhesives and mechanical load cycling on the micromorphology of the resin-dentin interdiffusion zone (of sound and caries affected dentin). The investigation considered two different Zn-doped adhesive approaches and evaluated the interface using a doubled dye fluorescent technique and a calcium chelator fluorophore under a confocal laser scanning microscopy. Sound and carious dentin-resin interfaces of unloaded specimens were deficiently resin-hybridized, in general. These samples showed a rhodamine B-labeled hybrid layer and adhesive layer completely affected by fluorescein penetration (nanoleakage) through the porous resin-dentin interface. It was thicker after phosphoric acid-etching and more extended in carious dentin. Zn-doping promoted an improved sealing of the resin-dentin interface, a decrease of the hybrid layer porosity, and an increment of dentin mineralization. Load cycling augmented the sealing of the Zn-doped resin-dentin interfaces, as porosity and nanoleakage diminished, and even disappeared in caries-affected dentin substrata conditioned with EDTA. Sound and carious dentin specimens analyzed with the xylenol orange technique produced a clearly outlined fluorescence when resins were Zn-doped, due to a consistent Ca-mineral deposition within the bonding interface and inside the dentinal tubules. It was more evident when load cycling was applied on specimens treated with self-etching adhesives that were Zn-doped. Micropermeability at the resin-dentin interface diminished after combining EDTA pretreatment, ZnCl2-doping and mechanical loading stimuli on restorations. It is clearly preferable to include the zinc compounds into the bonding constituents of the self-etching adhesives, instead of into the primer ingredients. The promoted new mineral segments contributed to reduce or avoid both porosity and nanoleakage from the load cycled Zn-doped resin dentin interfaces. EDTA+SB-ZnCl2 or SEB·Bd-Zn doping are preferred to treat caries-affected dentin surfaces. ZnO-doping encouraged for etch-and-rinse adhesives.

Improved Sealing and Remineralization at the Resin-Dentin Interface After Phosphoric Acid Etching and Load Cycling.

The purpose of this study was to investigate micro-morphology of the resin-dentin inter-diffusion zone using two different single-bottle self-etching dentin adhesives with and without previous acid-etching, after in vitro mechanical loading stimuli. Extracted human third molars were sectioned to obtain dentin surfaces. Two different single-bottle self-etching dentin adhesives, Futurabond U and Experimental both from VOCO, were applied following the manufacturer's instructions or after 37% phosphoric acid application. Resin-dentin interfaces were analyzed with dye assisted confocal microscopy evaluation (CLSM), including the calcium-chelation technique, xylenol orange (CLSM-XO). CLSM revealed that resin-dentin interfaces of unloaded specimens were deficiently resin-hybridized, in general. These samples showed a Rhodamine B-labeled hybrid complex and adhesive layer completely affected by fluorescein penetration (nanoleakage) through the porous resin-dentin interface, but thicker after PA-etching. Load cycling promoted an improved sealing of the resin-dentin interface at dentin, a decrease of the hybrid complex porosity, and an increment of dentin mineralization. Load cycled specimens treated with the XO technique produced a clearly outlined fluorescence due to consistent Ca-mineral deposits within the bonding interface and inside the dentinal tubules, especially when the experimental adhesive was applied.

Does endodontic post space irrigation affect smear layer removal and bonding effectiveness?

The effect of different post space irrigants on smear layer removal and dentin bond strength was evaluated. Sixty-six extracted sound maxillary central incisors were endodontically treated. After post space preparation, the teeth were assigned to three groups of 22 teeth each. The teeth of these three groups were irrigated for 1 min with 17% ethylenediaminetetracetic acid (EDTA) (group 1), 5.25% sodium hypochlorite (NaOCl) (group 2), or 0.9% sodium chloride (NaCl) (group 3). In each group, eight specimens were split longitudinally for smear layer evaluation, and the other fourteen specimens were filled with a self-etching adhesive system (Panavia F). Four of 14 specimens of each group were prepared for evaluation of the resin-dentin interdiffusion zone (RDIZ) and resin tags, and the other 10 specimens were serially sectioned for push-out test analysis. Smear layer removal and bond strength were affected by different post space irrigants. EDTA removed the smear layer extremely effectively and, as a result, improved the bond strength at each region (apical, middle, and coronal) of the roots. Resin tag formation and the RDIZ were also affected by different irrigants and in accordance with bond strength. Therefore, removal of the smear layer use a self-etching luting system plays an important role in bonding effectiveness.

Short Resin-posts Bonding to Primary Dentin. Microleakage and Micro-morphological an in vitro study.

The aim of this in vitro study was to evaluate the adhesion of two bonding systems (Single Bond and Adper Prompt L Pop, 3M ESPE) to short resin posts in the root dentin of primary teeth. Statistical analysis (Mann Whitney) revealed that there were no statistically significant differences between the materials (p= 0.75), but the Single Bond group presented a wider resin-dentin inter-diffusion zone (RDIZ). Both groups showed long resin tags. It was concluded that although Single Bond produced a wider adhesive interface than Adper Prompt L Pop, leakage levels occurred in both systems.

Overestimating hybrid layer quality in polished adhesive/dentin interfaces.

The most popular techniques for determining the quality of the hybrid layer (HL) have relied on morphologic characterization of the polished adhesive/dentin (a/d) interfaces before and after acid-bleach chemical treatment. Using these techniques, the existence of smooth, acid-resistant layers has been consistently reported for most adhesive systems. The purpose of this study was to determine whether popular specimen preparation techniques that include polishing and acid-bleach treatment modify the a/d interface, mask the complexity of the HL, and lead to inaccurate assessment of the quality of the HL. To understand the impact of specimen preparation techniques on the morphology of the resin-dentin interface, polished and unpolished specimens from the same tooth were closely compared after different acid-bleach chemical treatment procedures. Two one-bottle adhesives, that is, 3M Single Bond and Pulpdent UNO, exhibiting distinct differences in hydrophilic/hydrophobic composition, were used in this investigation. Using specimens from the same tooth, the effect of chemical treatments on the morphology of the resin-dentin interdiffusion zone and the differences in the morphology of polished and unpolished specimens after these same treatments were studied with scanning electron microscopy. It was shown that conventional specimen preparation techniques that include polishing and acid-bleach treatment can adversely affect and even obscure the structural detail of the a/d interface in specimens that possess a porous HL. The results indicated that the Pulpdent UNO/dentin interface had better quality than the 3M Single Bond/dentin interface. The difference in the quality of HL can be attributed to factors such as compositional differences that impact the adhesive interaction with water, that is present within the substrate during wet bonding. The inability of the conventional acid-bleach procedure to reveal the differences in the scanning electron microscopy interfacial morphology was overcome in this investigation by using a multistep technique.

Influence of a microbrush on bonding fiber post into root canals under clinical conditions.

The objective of this clinical report was to evaluate the effectiveness of a microbrush as a carrier of priming-adhesive solution in formation of resin tags, adhesive lateral branches, and resin-dentin interdiffusion zone (RDIZ) when the brush was used to bond fiber posts under clinical conditions. Twenty endodontically treated teeth, already scheduled for extraction for endodontic or periodontal reasons, were selected for this study. The patients were informed, and their written consent was obtained. The samples were randomly divided into 2 groups of 10 samples each. In group 1, One-Step (Bisco, Schaumburg, Ill) was applied with a brush with Duo-Link resin cement (Bisco). In group 2, One-Step was applied with a microbrush with Duo-Link resin cement (Bisco). Use of the adhesive systems and resin cements was strictly according to manufacturers' instructions. The priming-adhesive solution was light-cured before the dual resin cement and the post were placed. Twenty Aestheti-Plus posts (white quartz fiber posts; RTD, St. Egreve, France) were used. A week after application, the root samples were extracted and processed for SEM observations. Both adhesive systems showed RDIZ and resin tag and adhesive lateral branch formation. In Group 2 samples, RDIZ morphology was easily detectable and uniform along root canals. Also, resin tag formation was well represented in all thirds. In group 1 samples, resin tag formation at the apical third and RDIZ formation was less evident. Statistically significant differences were found among the two groups at the apical third. The microbrush permitted a more uniform RDIZ and resin tag formation along the entire length of the canal than did the standard brush. The microbrush can be routinely used for bonding fiber posts into root canal preparations.

An SEM evaluation of several adhesive systems used for bonding fiber posts under clinical conditions

Objectives: The objective of this investigation was to evaluate the effectiveness of three ‘one-bottle’ and two ‘three step’ adhesive systems (as controls) in the formation of resin tags, adhesive lateral branches and a resin dentin interdiffusion zone (RDIZ) when used to bond fiber posts under clinical conditions. This study was performed using standardized SEM observations and scoring resin tag formation and density. Methods: Fifty root canal treated teeth, already scheduled for extraction for endodontic or periodontal reasons, were selected for this study. The patients were informed and their written consent was obtained. The samples were randomly allocated to five groups of ten samples each. Group 1: All Bond 2 with C & B (Bisco); Group 2: Scotchbond Multipurpose Plus with Opal Luting Composite (3M); Group 3: Scotchbond 1 in combination with Rely X ARC resin cement (3M); Group 4: One-step with C & B resin cement (Bisco); Group 5: All Bond Experimental with Post Cement HI–X (Bisco). The adhesive systems and resin cements were used strictly according to the manufacturers’ instructions. The priming-adhesive solution of each ‘one-bottle’ system was light-cured before placing the resin cement and the post. Fifty Aestheti-Plus posts (white quartz fiber posts, RTD, France) were used. A week later, the roots were extracted and processed for SEM observations. Results: All the adhesive systems showed a RDIZ and resin tag and adhesive lateral branch formation. Microscopic examination of the restored interfaces of Groups 1 and 2 showed a higher percent of RDIZ than those found in samples of Groups 3, 4 and 5. RDIZ morphology was easily detectable and uniform in the first two thirds of the root canals, whilst in the apical third the RDIZ was not uniformly present. Resin tag morphology and formation were significantly more detectable in the cervical and middle areas than in the apical zone. No statistically significant differences were found among the five groups coronally, while in the apical and middle thirds two ‘one-bottle’ systems (Groups 3 and 4) showed significantly less resin tags than the control Groups 1, 2 and the experimental Group 5. No statistically significant differences were found among the three ‘one-bottle’ systems in the three evaluated areas. The standardization of SEM observations and scoring resin tag formation allowed statistical evaluation. Conclusions: The ‘three step’ adhesive systems can create a wider micromechanical interlocking between adhesive materials and etched dentin than ‘one-step’ systems.

Comparison Between Two Clinical Procedures for Bonding Fiber Posts into a Root Canal: A Microscopic Investigation

The purpose of this study was to evaluate the influence of two brushes used as carriers of a primer-adhesive solution as to the formation of resin tags, adhesive lateral branches, and a hybrid layer when used to bond translucent fiber posts. Twenty endodontically treated teeth, extracted for periodontal reasons, were used. The samples were randomly divided into two groups of 10 samples each (Group 1: Microbrush + Scotchbond 1 + Rely X ARC resin cement; Group 2: small plastic brush + Scotchbond 1 + Rely X ARC resin cement). The adhesive system and resin cement were used strictly following manufacturers' instructions. The priming-adhesive solution of the one-bottle system was light-cured before placing the resin cement and the post. Twenty translucent fiber posts were used. After luting procedures, root samples were processed for SEM observations. The adhesive system showed a resin dentin interdiffusion zone (RDIZ), resin tag, and adhesive lateral branch formation. Microscopic examination of restored interfaces of group 1 showed a higher percentage (p < 0.05) of RDIZ than those found in samples of group 2. In group 1 samples, RDIZ morphology was well detectable and uniform in all thirds of the root canals. In group 2, RDIZ was not visible in the apical third. No statistically significant differences were found among the two groups coronally and at the middle third, but the apical third of group 1 showed significantly more resin tag formation than group 2. The characteristic reverse cone shape of resin tags was always noted in the coronal and middle third of the root canals of both groups and in the apical third of group 1. In the apical third of group 2 root canals, the resin tags showed a less uniform morphology and a shorter length than those found in the other observed thirds.

Efficacy of different adhesive techniques on bonding to root canal walls: an SEM investigation

Objectives: Recently, several adhesives have been proposed for bonding fiber posts into root canals. The aim of this study was to evaluate the influence of four adhesive procedures in resin tag, adhesive lateral branch and resin dentin interdiffusion zone (RDIZ) formation when used to bond fiber posts. Method: Forty anterior teeth, extracted for periodontal reasons and endodontically treated, were selected for this study. The samples were randomly divided into four groups of ten samples each. Group 1: One Step applied with the small brush provided by the manufacturer and LC (Light-cured before resin cement application)+Dual Link resin cement; Group 2: One Step applied with a thin microbrush LC+Dual Link resin cement; Group 3: One Step applied with a small brush (Not light-cured)+Dual Link resin cement; Group 4: All Bond 2+C & B resin cement (as control). In Group 2 and 4 the adhesive system and resin cement were used strictly following manufacturers’ instructions. In Group 1, One Step was applied using a thin microbrush, while in the other groups by a small brush. In Group 1 and 2 the priming-adhesive solution of the ‘one-bottle’ system was light-cured before placing the resin cement and the post, whereas in Group 3 the adhesive/resin cement combination was light cured through the translucent post. Forty translucent posts (RTD, France) were used. A week later, the root samples were processed for SEM observations. Results: Microscopic examination of restored interfaces of Group 1 showed a higher % ( P<0.05) of RDIZ than those found in samples of Group 2, 3 and 4. In Group 2, 3 and 4 samples RDIZ morphology was well detectable and uniform in the first two thirds of root canals while in the apical third the RDIZ was not uniformly present. No statistically significant differences were found among the groups coronally, whereas apical and middle thirds of Group 1 showed significantly more resin tags than the other three Groups. In the apical third of Group 2, 3 and 4 samples, the resin tags showed a less uniform morphology and a shorter length than those found in the other two thirds. Significance: A microbrush might clinically be used for bonding fiber posts into the root canal. When a microbrush was used, the bonding mechanism created between root canal dentin and bonding system was uniform along canal walls and more predictable.

Heterogeneous distribution of single-bottle adhesive monomers in the resin–dentin interdiffusion zone

The purpose of this study was to investigate whether monomer separation occurs in single-bottle adhesives applied on acid-etched dentin surfaces. Smear-layer covered dentin specimens produced from sound premolars, were acid-etched and analyzed by micro-MIR FTIR spectroscopy, before and after treatment with the single-bottle adhesives One-Step, Prime and Bond 2.1, Scotchbond 1 and Syntac-Sprint. The difference spectra (etched, and primed minus etched of the same dentin surfaces) were plotted and compared with original adhesive spectra. The C=C/C...C (aromatic adhesives) and C=C/C=O (aliphatic adhesives) peak area ratios were used to evaluate the extent of monomer separation relative to original adhesive spectra at the uppermost 2 microm of the resin-dentin interdiffusion zone. Three dentin specimens were used for each adhesive. One-way ANOVA and Newman-Keuls tests were performed to assess the statistically significant differences (alpha=0.05). All the adhesives demonstrated separation of monomer components on etched dentin ranging in mean values from 68.7 to 81.9% relative to reference. High molecular weight hydrophobic (i.e. BisDMA, BisGMA, BisGMA adducts) and hydrophilic monomers (i.e. BPDMA) predominated at the region probed. Prime and Bond 2.1 demonstrated the highest extent of monomer separation. Heterogeneous monomer distribution following application to etched dentin may affect the curing performance of single-bottle adhesives within the resin infiltrated region and consequently, the mechanical and chemical stability of the network formed.

Confocal and scanning electron microscopic study of teeth restored with fiber posts, metal posts, and composite resins

Forty-two single-rooted lower premolars, extracted for periodontal reasons, were endodontically treated and divided into 7 groups of 6 teeth each. In five of the groups, three different types of carbon fiber posts, quartz fiber posts, and titanium posts were used in combination with All Bond 2 dental adhesive. In two groups, two types of carbon fiber posts were also cemented with Panavia 21 dental adhesive. After 3 wk storage in saline, the teeth were longitudinally sectioned; one half was observed using confocal microscopy and the other by scanning electron microscopy. The specimens were evaluated for the presence of a resin dentin interdiffusion zone for the presence of voids at post-resin-dentin interfaces and for the determination of the fiber posts' structure. Upon examination with the confocal microscope, the interfaces of teeth restored with All Bond 2 showed a higher percentage (p < 0.05) of resin dentin interdiffusion zone than those treated with panavia. The fiber size and the post structure were similar in all the fiber posts observed. Some voids were present inside the fiber post structure.

Human dentin and the dentin-resin adhesive interface

Dentin, the inner hard tissue of teeth, is a complex hydrated composite and forms the substrate for much of restorative dentistry. Current efforts to improve restorative and preventive dentistry involve the development of effective bonds to this tissue. Modern bonding techniques involve etching the dentin to remove the mineral portion, leaving a collagen network that can be infiltrated with a monomer and polymerized in place to form a mechanical bond. The objective of this study was to investigate the nature of the interfacial zone, called the resin-dentin interdiffusion zone, using scanning electron microscopy for characterization and thickness measurements, X-ray tomographic microscopy for fracture characteristics and atomic force microscopy for the local modulus and hardness variations.

In vitro interfacial relationship between human dentin and one-bottle dental adhesives

Objectives One-bottle dentin adhesives combine primer and adhesive resin into a single solution. This study was conducted to determine the bond strengths to dentin of four one-bottle bonding systems and to evaluate their SEM interfacial morphology. The hypothesis to be tested was that the water-based bonding system would produce lower bond strengths and less complete penetration into dentin than other bonding systems that are dissolved in organic solvents. Methods Forty extracted molars were ground to expose middle dentin and were randomly assigned to four groups (n = 10): Group 1 - Experimental Single Bond (3M Dental Products Division); Group 2 - Prime&Bond 2.1, pre-launch version (Dentsply DeTrey); Group 3 - Syntac Single-Component (Vivadent); Group 4 - Tenure Quik with Fluoride (Den-Mat Co.) The surfaces were treated according to manufacturers' instructions. After 24 h in water, the specimens were thermocycled, and the bond strengths were measured in shear. The data were analyzed with ANOVA and Duncan's test at a confidence level of 95%. Further, the adhesives were also applied to 600 pm thick dentin disks. After preparing polished cross sections, the bonded interfaces were demineralized, deproteinized, and observed under a FE-SEM. The morphological appearance of the resin-dentin interface surfaces was compared by screening the entire resin-dentin interface for each specimen. Results Two morphological characteristics were evaluated:1) the depth of resin penetration into the tubules and 2) the thickness and density of the resin-dentin interdiffusion zone. Single Bond showed statistically higher mean shear bond strengths (p < 0.001) compared to the other three materials. Specimens prepared with Syntac Single-Component and Prime&Bond 2.1 were ranked in the intermediary Duncan's grouping. Specimens bonded with Tenure Quik with Fluoride exhibited the lowest mean shear bond strength. All materials penetrated and hybridized dentin. Single Bond formed a thick layer of adhesive resin on the top of the interdiffusion area without debonding, whereas some areas of debonding were observed on the top of the hybrid layers for Prime&Bond 2.1 and Syntac Single-Component. For the water-based adhesive Syntac Single-Component, the interdiffusion zone displayed a thick filigree pattern, containing scattered open spaces between the resin-enveloped collagen fibers. Tenure Quik with Fluoride did not thoroughly infiltrate the demineralized dentin zone, resulting in wide gaps in all specimens. Prime&Bond 2.1 formed the shortest resin tags, whereas Syntac Single-Component formed the longest resin tags. Significance Bonding to dentin remains unpredictable using one-bottle bonding systems. The chemistry of each individual material may be more important than the type of solvent.

In vivo resin-dentin interdiffusion and tag formation with lateral branches of two adhesive systems

The close contact of the primer and the conditioned dentin is critical in the bonding of resin composites to dentin. In this study two different adhesive primers were tested in vivo with a separate conditioning procedure (Scotchbond Multipurpose) and a self-etching primer (Clearfil Liner Bond 2). The formation of lateral branches of tubule tags was investigated to substantiate the effectiveness of infiltration as a contribution to retention. Scanning electron microscopy revealed the formation of a resin-dentin interdiffusion zone and penetration into the lateral canals of the tubules for both primers. The resin tags with lateral branches were observed primarily at the floor of the class II cavities. In vivo effectiveness of self-etching priming was demonstrated.

Morphologic aspects of the resin-dentin interdiffusion zone with five different dentin adhesive systems tested in vivo

The new generation of enamel dentin adhesive materials provides removal of the smear layer, inducing structural changes in the dentinal surface and creating a retentive interdiffusion zone or hybrid layer between the two substrates. Some studies have demonstrated hybrid layer formation in in vitro samples, but few articles have described it in in vivo specimens. The hybrid layer forms in peritubular and intertubular treated dentin and improves adhesion between tooth surface and adhesive resins. This in vivo study investigated the formation of a hybrid layer by use of five different enamel dentin adhesive systems. The dentin adhesives systems were tested on flat dentin preparations made on vestibular surfaces of periodontally compromised teeth. The sample teeth were extracted immediately after the resin was cured. Half of the samples were used to visualize the hybrid layer and the other half to observe the morphology of the resin tags by use of scanning electron microscopy. All the tested products formed a hybrid layer. In many areas of samples of Gluma 2000, Scotchbond Multipurpose, All Bond 2, and Super Bond D Liner systems, characteristic reverse cone-shaped tags were visible. Resin tags produced by Clearfil Liner Bond adhesive were narrower at the apertures of tubules than those of the other four adhesive materials. Morphology of the hybrid layer and of the resin tags of these samples were similar to in vitro samples observed in other studies.

Assessment by nano-indentation of the hardness and elasticity of the resin-dentin bonding area.

The hardness and Young's modulus of the successive layers across a resin-dentin bonding area were determined by nano-indentation for four commercially-available dentin adhesive systems, of which two were also applied with a different conditioning agent. With a computer-controlled nano-indentation technique, minute triangular indentations were made within a small area of a few micrometers' diameter at a load of a few milli-Newtons. The load and displacement of the indenter were continuously monitored during the loading-unloading sequence, so hardness and Young's modulus could be computed as a function of the indenter geometry and the applied load. The hardness of the resin-dentin interdiffusion zone was significantly lower than that of unaltered dentin. A gradient of moduli of elasticity was observed from the rather stiff dentin over a more elastic resin-dentin interdiffusion zone and adhesive resin layer to the restorative composite. That gradient was more substantial in those systems that produced relatively thick adhesive resin layers or supplementally provided a filled low-viscosity resin as an intermediate layer between the adhesive resin and the bulk restorative composite. Such an elastic bonding area might have a strain capacity sufficient to relieve stresses between the shrinking composite restoration and the rigid dentin substrate, thereby improving the conservation of the dentin bond and, as a consequence, the marginal integrity and retention of the restoration.

Comparative SEM and TEM examination of the ultrastructure of the resin-dentin interdiffusion zone.

The resin-dentin interdiffusion zone produced by a dentin-adhesive system that removes the smear layer and concurrently decalcifies superficial dentin was morphologically examined by both scanning and transmission electron microscopy. Cross-sectioned resin-bonded dentin discs were etched with an argon-ion beam to make the resin-dentin interface observable by SEM. For the TEM examination, the sections were partly decalcified by an aqueous EDTA solution to facilitate ultramicrotomy and to disclose the ultrastructure of the interdiffusion zone. Both SEM and TEM confirmed the presence of the resin-dentin interdiffusion zone as the junction between the deep unaltered dentin structure and the restorative resin. Within the interdiffusion zone, three sublayers with characteristic ultrastructure and staining were identified by TEM. An upper diffuse black layer contained few structural features. Underneath, partially-altered collagen fibrils were closely packed, mostly running parallel with the interface and perpendicular to the dentinal tubules. Their outline was electron-dense, forming tunnel-like structures. At the base of the upper layer, several stained projections were found to bulge out into the underlying collagen network and appeared to be confined by obstructive, parallel-running collagen fibrils. Finally, the third dense layer, containing hydroxyapatite crystals, demarcated the superficially demineralized dentin layer from the deeper unaltered dentin. Resin diffusion into the decalcified dentin surface layer was evident, but diminished with depth, presumably reducing deeper resin impregnation into the interfibrillar spaces. The citric acid dentin-pretreatment probably caused denaturation of the superficial collagen fibrils. Its decalcifying effect gradually weakened with depth, leaving behind hydroxyapatite crystals at the base of the interdiffusion zone.(ABSTRACT TRUNCATED AT 250 WORDS)

Morphological aspects of the resin-dentin interdiffusion zone with different dentin adhesive systems.

Cross-sections of resin-dentin interfaces were etched with an argon-ion beam to make their substructure detectable by scanning electron microscopy. The dentin adhesive systems were categorized morphologically into three groups, and an attempt was made to clarify their adhesive mechanism. The first group of products removed the smear layer. The argon-ion bombardment clearly disclosed a hybrid or resin-impregnated dentin layer. It is hypothesized that conditioning with acidic or chelating agents demineralized the dentin surface-layer to a certain depth, leaving behind a collagen-rich mesh-work. Hydrophilic monomers are then believed to alter this collagen-fiber arrangement in a way that facilitates penetration of the adhesive resin, resulting in a mechanical, intermingled link between collagen and the adhesive resin. The second group preserved the smear layer. In this case, the dentinal tubules were obliterated with globular particles at their orifices and remained patent underneath these smear plugs. This type of adhesive system aims at the incorporation of the smear layer into the hydrophilic monomers, which have an affinity for the organic and/or inorganic components of the underlying dentin. Finally, a third, small group only partly dissolved the smear layer, creating a thin resin-impregnated dentin layer and a resin-impregnated smear plug. This study clearly showed that the application of recent adhesive systems induced structural changes in the dentin surface morphology, creating a retentive interface, called the inter-diffusion zone, between the deep, untouched dentin layers and the composite filling material. This resin-dentin interdiffusion zone offers bonding sites for copolymerization with the resin composite and, concurrently, might have protective potential for the pulp tissues.