The purpose of this study was to observe the morphologic change of dentinal surface, adhesion in interface between dentin and bonding agents, and penetration pattern of resin tags into dentinal tubles according to bonding procedure of ONE-STEP universal adhesive system. Ten extracted human molars were mounted in dental stone and sectioned to expose mid-coronal occlusal dentin and again sectioned tooth crown apically. Specimens were randomly assigned to three groups for dentin conditioning with 32% phoshoric acid, two coats of bonding agents after dentin conditioning, and bond of composite resin. The surfaces of dentin were treated with etch ant and applied bonding agent, and bonded composite resin according to the directions of manufacturer. Specimens which were boned composite were sectioned longitudinally for observing interfaces between resin and dentin. Two of specimens which were sectioned longitudinally were immersed in 6 N HCL for 30 seconds and 1% NaOCL for 12 hours to partially demineralize and deproteinize the dentin substrate. Each specimen was mounted on a brass stub, sputter-coated with gold and observed under SEM. The result were as follows : 1. On the dentinal surface which was conditioned with 32% phosphoric acid. the smear layer was completely removed. orifices of dentinal tubules were opened 3-$5{\mu}m$ wide. and dentinal surface was irregular. 2. On the dentinal surface which was applied ONE-STEP. bonding agent. resin particles were observed on the orifices of dentinal tubules and intertubular dentin. 3. There were close adaptation between dentin and resin and were the pattern which composite invaded into dentin. 4. 1-$3{\mu}m$-wide hybrid layer was visible in the interface between dentin and resin. 5. Long and funnel shaped resin tags were observed in demineralized specimens. and the surfaces of tags were rough.
This study was executed to evaluate adaptability of dentin bonding agents to dentinal wall with measuring contraction gap on interface between cavity wall and composite resin by SEM study. 6 kinds of dentin bonding agents were investigated for this study : Gluma, Super Bond C & B, All bond 2, Scotchbond multipurpose, Scotchbond 2 and Clearfil photo bond. 30 of fresh extracted teeth were randomly selected and divided into 6 groups with each 5. The round shaped cavities with 3mm dia. and 1.5mm depth were prepared on cementoenamel junction of buccal surface of teeth. Dentin bonding agents were applied to cavity wall and then the composite resin was filled in the cavity. Specimens were sectioned longitudinally on buccal surface. Sectioned aspects of specimens were impressioned with rubber base materials and finally precise replica were made of epoxy resin poured in negative impression. Contraction gaps were examined on interface between cavity wall and composite resin under condition of 200 and 2000 magnification of SEM. The results were as follows. 1. There were no gap on interface between enamel and composite resin in all specimens, but gaps were mainly exhibited on apical side of lateral wall of dentin of cavity. 2. In Gluma, 2 cases of 5 specimens exhibited excellent adaptation to the cavity wall, indicating no gaps on interface between cavity wall and composite resin. The other specimens showed gaps with range of $0{\sim}15{\mu}m$ width. 3. In Super Bond C & B, gaps with range of $0{\sim}10{\mu}m$ width were mainly exhibited on apical side of lateral wall of dentin of cavity. 4. In All bond 2, all specimens showed the most exellent adaptation to cavity wall when compared to the other materials, indicating no gap interface between cavity wall and composite resin. 5. In Scotchbond multipurpose, gaps with range of $0{\sim}10{\mu}m$ width were locally located on cavity wall. 6. In Scotchbond 2, all specimens showed great amount of gap with range of $5{\sim}25{\mu}m$, indicating the worst adaptation to cavity wall compared to the other materials. 7. In Clearfil photo bond, 2 case of 5 specimens exhibited exellent adaptation to cavity wall, indicating no gap. the other specimens showed gap with range of $0{\sim}15{\mu}m$ width on inferface between cavity wall and composite resin.
Park, Jong-Duk;Lee, Yong-Woo;Ohn, Yeong-Suck;Lee, Kwang-Won
Restorative Dentistry and Endodontics
/
v.23
no.1
/
pp.443-460
/
1998
The purpose of this study was to estimate the changes of tensile bond strength according to the difference in lining materials and lining area. Seventy non-carious extracted human molars were used in the present study, and they were randomly assigned into 2 experimental groups according to the difference in lining materials. Each experimental group was subdivided into 3 groups according to the difference in lining area. Circular cavities were prepared on the dentin surface to a diameter of 1.5mm, 2.0mm, 2.5mm and the prepared cavities were filled with Fuji II LC( Glass Ionomer Cement : GIC) or Dycal. Dentin specimens without circular cavity were used as control group. The primer and bonding agent of All-Bond 2 and composite resin (Z-100, 3M Dental Products, U. S. A.) were applied to the exposed dentin surface with or without lining. Tensile bond strengths for the experimental specimens were then measured. To examine the interface between dentin and liner & between liner and composite resin, two specimens from each group were fabricated and observed under the SEM. The results were as follows. 1. Tensile bond strength for the specimens lined with GIC was higher than that for specimens lined with Dycal. However, there was no significant difference between two groups(p>0.05). 2. Tensile bond strength for the specimens lined with GIC in a diameter of 1.5mm(GIC-1.5mm lining group) was statistically higher than that for the GIC-2.0mm lining group and GIC-2.5mm lining group(p<0.05). 3. Tensile bond strength for the specimens lined with Dycal in a diameter of 2.5mm (Dycal-2.5mm lining group)was statistically lower than that for Dycal-1.5mm lining group and Dycal-2.0mm lining group(p<0.05). 4. It was possible to observe the good adhesion of the resin composite to the GIC and the presence of a fissure between GIC and dentin all along the interface. Interfacial gaps of 7.2-$72.2{\mu}m$ between GIC and dentin were observed. The interfacial gap between GIC and dentin at the cavity base was greater. However, the gap was gradually decreased toward the occlusal portion. 5. It was possible to observe the poor adhesion of the resin composite to the Dycal. The detachment of Dycal was occurred all along the composite resin-Dycal interface, and the gaps of 2.0-$30.1{\mu}m$ were formed. In all the specimens, polymerization shrinkage of resin composite caused the detachment of Dycal from the body of Dycal. At a Dycal-dentin interface. it was possible to observe the good adhesion. but poor adhesion with interfacial gap of 2.9-$26.8{\mu}m$ was observed partially.
The purpose of this study was to evaluate on the interfacial morphology between dentin and restorative materials. In this in vitro study, the cavity wall restorated with 3 different kinds of tooth colored restorative materials [resin-modified Glass Ionomer cement (Fuji II LC), composite resin (Z-100), compomer (Dyract)]. The thirty extracted human molar teeth without caries and/or restorations are used. The experimental teeth were randomly divided into three groups of ten teeth each. In each group, Wedge shaped cavities (width: 3mm, length: 2mm, depth: 1.5mm) were prepared at the cementoenamel junction on buccal and lingual surfaces. The adhesive of composite resin were mixed with rhodamine B. Primer of composite resin, Prime & Bond 2.1 of Dyract and liquid of Fuji II LC were mixed with fluorescein. In group 1, the cavity wall was treatment with dentin conditioner, and then restorated with Fuji II LC. In group 2, the cavity wall was treatment with Prime & Bond 2.1 and then restorated with Dyract. In group 3, the cavity wall was etching with 10% maleic acid, applied with primer and bonding agent and then restorated with Z-100. The interface between dentin and restorative materials was observed by fluoresence imaging with a confocal laser scanning microscope. The results were as follows : 1. In Glass ionomer group, adaptation of resin modified Glass-ionomer restoration against cavity wall is tight, but the crack formed inside of restoration were observed. 2. In Dyract group, the penetration of resin tag is shorter and the width of hybrid layer is narrower than composite resin group. 3. In Z-100 group, primer penetrated deeply through dentinal tubule. Also bonding agent was penetrated along the primer, but the penetration length is shorter than primer part, and in 3-D image, the resin tag is conical shape and lateral branch is observed.
The purpose of this study was to evaluate the effect of moistening and air-drying of acid conditioned dentin and enamel on the marginal microleakage. In this study, Class V cavity were prepared on both buccal and lingual surface of sixty extracted human premolars with cementum margin. These specimens were randomly devided into three groups and three dentin adhesives(Scotchbond Multi-Purpose, All bond 2, Prisma Universal Bond 3) were applied to each group. The specimens in each group were subdevided into four groups (Wet/primed, Dry/primed, Wet/not primed, Dry/not primed) and the etched dentin and enamel surface were treated these four surface treatments prior to the placement of a bonding agent or adhesive. Wet/primed group was simply blot-dried with a damp facial tissue before primer placement ; Dry/primed group was air dried for 30 seconds before the placement of a primer ; Wet/not primed group and Dry/not primed group were not primed after blot dried and air dried for 30 seconds each group. The bonding agent and composite resin were applied for each group. All specimens were exposed to 500 cycle of thermal stress. Specimens were placed in a silver nitrate solution and then sectioned buccolingually through the center of the restoration. The dye penetrations of the specimens were observed with a stereo microscope. The statistical test were applied to the results using a one way analysis variance (ANOVA) and Duncan's multiple range test. The aspects of silver ion penetration into the resin/dentin interface were examined under scanning electron microscopy. The results were as follows. 1. In all groups, the enamel margin showed significantly lower leakage value than the cementum margin (p<0.05). 2. Regardless of various surface treatment and dentin adhesives, there was no significant difference at the enamel margins (p>0.05). 3. At the dentin margins, the leakage values of Dry/not primed group showed significantly higher than that of the other groups (p<0.05). The leakage values of Wet/primed group showed significantly lower than that of the other groups, but, there was no significant difference between Wet group and Dry group. 4. There was no significantly difference between the dentin adhesives regarding the surface treatments in all groups(p>0.05). 5. On the backscatterd scanning electron microscopy observation, the penetration of the silver ion occured at the bonding resin/dentin interface. In the Wet/primed group, resindentin hybrid zone and resin penetration into the dentin was observed. The resin tags were compactively formed to a thickness of $3\sim4{\mu}m$ at the upper part of dentinal tubules. In the Dry/primed group, the thickness of the hybrid zone and the diameter, depth of the resin tags diminished. In the Non-primed groups, the hybrid zone was not identified and few resin tag was observed. There was the gap formation in the resin/dentin interface.
In the case of CAD/CAM ceramic inlay restorations, if isthmus width is widened too much, it may cause fracture of remaining tooth structure or loss of bonding at the luting interface because of excessive displacement of buccal or lingual cusps under occlusal loads. So to clarify the criterior of widening isthmus width, this study was designed to test the tensile bond strength and bond failure mode between dentin and ceramic cemented with luting composite resin cements. Cylindrical ceramic blocks(Vita Cerec Mark II, d=4mm) were bonded to buccal dentin of 40 freshly extracted third molars with 4 luting composite resin cements(group1 : Scotchbond Resin Cement/Scotchbond Multi-Purpose, group2 : Duolink Resin Cement/ All-Bond 2, group3: Bistite Resin Cement/Ceramics Primer, and group4:Superbond C&B). Tensile bond test was done under universal testing machine using bonding and measuring alignment blocks(${\phi}ilo$ & Urn, 1992). After immersion of fractured samples into 1 % methylene blue for 24 hours, failure mode was analysed under stereomicroscope and SEM. Results: The tensile bond strength of goup 1, 2 & 4 was $13.97{\pm}2.90$ MPa, $16.49{\pm}3.90$ MPa and $16.l7{\pm}4.32$ MPa, respectively. There was no statistical differences(p>0.05). But, group 3 showed significantly lower bond stregnth($5.98{\pm}1.l7$ MPa, p<0.05). In almost all samples, adhesive fractures between dentin and resin cements were observed. But, in group 1, 2 & 4, as bond strength increased, cohesive fracture within resin cement was observed simultaneously. And, in group 3, as bond strength decreased, cohesive fracture between hybrid layer and composite resin cement was also observed. Cohesive fracture within dentin and porcelain adhesive fracture were not observed. In conclusion, although adhesive cements were used in CAD/CAM -fabricated ceramic inlay restorations, the conservative priciples of cavity preparation must be obligated.
The effect of moistening and air-drying of acid-conditioned dentin before priming on the formation of resin-dentin hybrid zone was investigated, Freshly extracted human molars were used and divided at random into 5 groups, Groups 1 - 3 consisted of specimens conditioned with 10 % phosphoric acid for 20 seconds; Group 1 served as a control in which the conditioned dentin was simply blot-dried with a damp facial tissue; Group 2 was air dried for 30 seconds ; Group 3 was air dried for 30 seconds and immediately remoistened for 10 seconds with air-water syringe. and then the specimen was blot-dried with a damp facial tissue. Groups 4-5 were not acid conditioned ; In group 4, the smear layer on the dentin was blot dried before primer placement; Group 5 was air dried only for 30 seconds, The acetone-based primer and bonding agent of All Bond 2 (Bisco. Inc., USA) and composite resin (Z-100, 3M Dental products, USA) were applied for acid conditioned dentin and non-conditioned dentin. The morphologic ultrastructure of resin-dentin hybrid zone was examined by the use of SEM and TEM. and the existence of inorganic material and analysis of Ca/P weight-percent ratio in the resin-dentin hybrid zone were revealed by the EDAX, The results were as follows : 1. In the moistened specimens from acid-conditioned groups, the resin penetrated about 3-$4{\mu}m$ into dentin and the denatured collagen smear layer was not present at the surface. The resin tag was formed to a thickeness of 3-$4{\mu}m$ at the upper part of dentinal tubule and compactively connected to each other by means of many lateral branching. 2. In the air-dried specimens from acid-conditioned groups, the resin penetrated about 2.0-$2.5\;{\mu}m$ into dentin and an upper thin black layer to a thickness of 30-35nm was identified between adhesive resin and demineralized collagen layer. The resin tag to have a diameter of $2.5{\mu}m$ was formed at the upper part of dentinal tubule. However the funnel shape of the tag was not notable compared to the moistened specimens. 3. In the remoistened specimens from acid conditioned groups, the resin penetrated about 2.0-$2.5{\mu}m$ into dentin and an upper black layer was not present. The resin tag at the upper part of dentinal tubule was formed less than $2{\mu}m$ and was weakly connected to each other by means of few lateral branching. 4. In the non-conditioned groups, the smear layer was formed to a thickness of $0.5{\mu}m$ at dentin surface. However, the resin-dentin hybrid zone was not identified by TEM. The evidence of resin penetration into intertubular and intratubular dentin did not show. 5. All the acid-conditioned groups showed that the detected calcium and phosphorus weight percent ratios at the $2{\mu}m$ upper portion from the resin-dentin interface into the resin were much higher than that at the $2{\mu}m$ lower portion from the resin-dentin interface to dentin. (P<0.01).
The purpose of this in vitro study was to evaluate dentin bonding by two different dentin bonding systems(DBS) using acetone based primer or adhesive [All Bond 2(AB2), One Step(OS)] when they were applied by wet or dry bonding technique. Morphology of resin-dentin interface and hybrid layer thickness(HLT) were investigated using Confocal Laser Scanning Microscope(CLSM) and compared to shear bond strength(SBS). 72 extracted sound human molars were randomly divided into 4 groups of 18 teeth each - Group 1.(AW); AB2 by wet bonding. Group 2(AD); AB2 by dry bonding. Group 3.(OW); OS by wet bonding, Group 4.(OD); OS by dry bonding. In 6 teeth of each group, notch-shaped class V cavities(depth 2mm) were prepared on buccal and lingual surface at the cementoenamel juction(12 cavities per group). To obtain color contrast in CLSM observation, bonding resins of each DBS were mixed with rhodamine B and primer of AB2 was mixed with sodium fluorescein. Prepared teeth of each group were treated with AB2, OS, respectively according to the manufacturer's instructions except for dentin surface moisture treatment after acid etching. In group 1 and 3, after acid etching, excess water was removed with wet tissue(Kimwipes), leaving consistently shiny, visibly hydrated dentin surface. In group 2 and 4, dentin surface was dried for 10 seconds at 1 inch distance. The treated teeth were then packed with composite resin(${\AE}$litefil) and light-cured. 12 microscopic samples($60{\sim}80{\mu}m$ thickness) of each group were obtained after longitudinal section and grinding(Exakt cutting and grinding system). Morphological investigation of resin-dentin interface and HLT measurement using CLSM were done. For measurement of SBS, remaining 12 teeth of each group were flattened occlusally to remove all enamel and grinded to 500 grit SiC(Pedemet Specimen Preparation Equipment). After applying DBS on the exposed dentin surface, composite resin was applied in the shape of cylinder, which has 5mm diameter, 1.5mm thickness, and light cured. SBS was measured using Instron with a crosshead speed of 0.5mm/min. It was concluded as follows, 1. HLT of AW(mean: $2.59{\mu}m$) was thicker than any other group, and followed by AD, OW, OD in descending order(mean; 2.37, 2.28, $1.92{\mu}m$). Only OD had statistically significant differences(p<0.05) to AW and AD. 2. There were intimate contact of resin and dentin at the interface in wet bonding groups, but gaps or irregular interfaces were observed in dry bonding groups. 3. The length, diameter, density of resin tags were various even in the same group without significant differences between groups and lots of adhesive lateral branches were observed. 4. There were no statistically significant difference of SBS between AB2 and OS, but SBS of wet bonding groups were significantly higher(p<0.05) than dry bonding groups. 5. There were no consistent relationships between HLT and SBS.
The purpose of this study was to evaluate the microleakage of 5 current dentin bonding systems which are composed of 2 multi-bottle systems(Scotchbond Multi-Purpose, All Bond2) and 3 one-bottle systems(Single bond, One-Step, Prime & Bond). In this in vitro study, class V cavities were prepared on buccal and lingual surfaces of sixty extracted human premolars and molars on cementum margin. The experimental teeth were randomly divided into six groups of 10 samples (20 surfaces) each, Group 1 : Scotchbond Multi-Purpose ; Group 2 : All Bond 2 ; Group 3 : Single Bond ; Group 4 : One-Step ; Group 5 : Prime & Bond ; Group 6 : no bonding agent(control). The bonding agent and composite resin were applied for each group following the manufacturer's instructions. After 500 thermocycling between $5^{\circ}C$ and $55^{\circ}C$, the 60 teeth were placed in 2% Methylene blue dye for 24 hours, then rinsed with tab water. The specimen were embedded in clear resin, then sectioned buccolingually through the center of restoration with a low speed diamond saw. The dye penetration on each of the specimen were then observed with a stereomicroscope at ${\times}20$. The results of study were statistically analyzed using the Student-Newmann-Keul's Methods and the Mann-Whitney Rank Sum Test. The resin/dentin interfaces were examined under Scanning Electron Microscopy. The results of this study were as follows. 1. None of the dentin bonding systems used in this study showed significant difference in leakage values at both the enamel and the dentin margins (P>0.05). 2. In all groups except the control, leakage value seen at the enamel margin was significantly lower than that seen at the dentin margin (P<0.05). 3. Compared to the control group, all the groups treated with dentin bonding systems showed significantly lower leakage value at both enamel and dentin margins (P<0.05). 4. In the SEM view, gaps were observed in the composite resin / dentin interface in group 6 where no dentin bonding agent was used, and in all the other groups (group 1, 2, 3, 4, 5) composite resin, hybrid layer, and dentin were seen to be closely adhering to each other where there were no leakages. Well-developed resin tags 3~100${\mu}m$ in length infiltrated dentinal tubules past the hybrid layer and a hybrid layer 1~5${\mu}m$ thick had developed between the dentinal surface and the composite resin surface.
Park, Sung-Taek;Moon, Joo-Hoon;Cho, Young-Gon;Ohn, Yeong-Suck
Restorative Dentistry and Endodontics
/
v.24
no.2
/
pp.381-391
/
1999
A new 5th generation adhesive system(ONE-STEP) has been supplied which operators can apply to conditioned tooth surfaces by one simplified step. The purpose of this study was to determine whether different methods of adhesive application and various air drying duration after applying adhesive affect the shear bond strength of composite resin to dentin, and to evaluate the adhesive pattern of composite resin and dentin under SEM. Seventy-seven extracted human molar teeth were cleaned and mounted in palstic test tubes. The occlusal dentin surfaces were exposed with Diamond Wheel Saw and smoothed with Lapping and Polishing Machine (South Bay Technology Co., U.S.A.). Teeth were randomly divided into 7 groups (n=11), In experimental A group, adhesive was applied to dentin with agitation for 20 sec. In experimental N-A group, adhesive were continuously applied to dentin for 20 sec. Also control and experimental 1, 2, 3, 4 groups were dried for 10, 0, 5, 20, 30 seconds after applying adhesive, respectively, Adhesives were light cured for 10 sec. A gelatin capsule 5mm in diameter was filled with Aelitefil$^{TM}$ composite resin, placed on the treated dentin surface and light cured for 40 see, from three sides, All specimens were stored in distilled water at room temperature for 24 hours. The shear bond strengths were measured using a universal testing machine(AGS-1000 4D, Japan) at a crosshead speed of 5mm/min. An one-way ANOVA and LSD test were used for statistical analysis of the data. For SEM evaluation, seven specimens were made and sectioned. Representive postfracture and seven specimens were mounted on brass stubs, sputter-coated with gold and observed under SEM. The results were as follows : 1. The shear bond strength of experimental A group which adhesive were applied to dentin with agitation was higher than that of experimental N-A group (continuous application), and there was significant difference between two groups (p<0.01). 2. The interface between composite and dentin according to different application methods showed close adaptation in experimental A group and showed tinny gap in experimental N-A group. 3. The shear bond strength accoding to various air drying duration was the lowest value(7.57${\pm}$2.60 MPa) in experimental 1 group, so there was significant difference between experimental 1 group and other four groups (p<0.05). But there was no significant difference of shear bond strength between four groups (p>0.05). 4. The interface between composite and dentin according to various air drying duration showed close adaptation in control group and tinny gap in experimental 3 and 4 groups. But experimental 1 and 2 groups showed $30{\mu}$ and 6 - $10{\mu}m$ thick gaps, respectively.
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