• Restorative Dentistry and Endodontics
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• v.21 no.1
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• pp.136-149
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• 1996

The effects of various All-Etching Agents (10% phosphoric acid, 10% maleic acid and 10 % citric acid) and 32 % phosphoric acid and varied etching time were evaluated by observing the morphology of the etched enamel surfaces using Scanning electron microscopy and by measuring the shear bond strength of a composite resin to human enamel. A total of 156 extracted premolar and molar teeth free of irregularities were employed in this study. Specimens for the observation of enamel morphology were divided into 12 groups of 3 teeth each, based on the type of etchant used and application time. After exposure to the etching agent specimens were washed air-dried and then glued to aluminum stubs and coated with a layer of gold for examination in the scanning electron microscope. Specimens for the evaluation of bond strength were divided into 12 groups of 10 teeth each also based on the type of etchant used and application time. After exposure to the etching agent the specimens were washed, air-dried and a thin layer of bonding agent was applied using a brush. Z 100 composite resin was light cured to the surface and stored at $37^{\circ}C$, 100% humidity for 7 days. An Instron Universal Testing Machine was used to apply a shearing force at $90^{\circ}$ angle from the enamel surface. It is concluded from this study that commercial All-etching agents can be used with a 15-second etching without adversely affecting retention of dental resin materials. At the same time, the acid concentration is probably a suitable compromise regarding the acid's function as a dentin demineralizing all-etch conditioning agent. The following results were obtained. 1. Specimens etched with 10 % citric acid showed a random superficial etching pattern which could not be related to prism morphology. 2. Specimens etched with 10 % and 32 % phosphoric acid and 10 % maleic acid showed a type I pattern in which core material was preferentially removed leaving the prism peripheries relatively intact or a type II pattern in which prism peripheries were preferentially removed. This delineation became more distinguished as etching time was increased. 3. All-Etching Agents and 32 % phosphoric acid showed a statistically significant higher shear bond strength at 15 seconds etching time.(p<0.05) 4. 10 % maleic acid and 32 % phosphoric acid exhibited a statistically significant higher shear bond strength than 10 % phosphoric and citric acid at 15 seconds etching time.(p<0.05).

• Restorative Dentistry and Endodontics
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• v.21 no.1
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• pp.227-241
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• 1996

The effect of collagen dissolution in acid conditioned dentin was morphologically examined by both scanning and transmission electron microscopy. 18 freshly extracted human molars and dentin bonding systems of All Bond 2, Scotchbond Multipurpose, Superbond D-Liner were used in this study. For SEM preparation, each 3 of ~ exposed dentin surfaces were acid conditioned by using various acids within the above three bonding systems respectively. After acid conditioning of the other 3 exposed dentin surfaces as above, they were treated with 1.7% NaOCl for 2 minutes. The remaining 3 dentin surfaces were acid conditioned and treated with 3.3 % NaOCl for 2 minutes. All of the specimens were then fixed in 4 % glutaraldehyde for 12 h at $4^{\circ}C$ and dehydrated in ethanols grades from 50 % to 100 %, then surface changes of the specimens were observed by using SEM. For TEM preparation, exposed dentin surfaces were acid conditioned with the same acid as SEM specimens and treated with 1.7%, 3.3 % NaOCl respectively, then applied with corresponding bonding agents. After the procedures were finished, composite resin were applied on the dentin surfaces and light cured. Small, rectangular sticks with end dimensions of approximately 1 by 1 mm were sectioned and further sample preparative techniques for transmission electron microscopy were performed in accordance with the procedures used for ultrastructural TEM observations of calcified tissues. The results were as follows : 1. In the 1.7 % NaOCl retreated specimens after acid conditioning, the porous dentin surface of intertubular dentin and wide opening of dentinal tubules were appeared. And there were fine irregularities on the intertubular dentin, indicating a clear difference as compared with the acid conditioned specimens. 2. In the 3.3% NaOCl retreated specimens after acid conditioning, the intertubular dentin was further eroded causing a more porous and wider opening of dentinal tubules. Moreover, sharp irregularities on the intertubular dentin were more evident than those of acid conditioned and 1.7% NaOCl retreated specimens. 3. In all of the acid conditioned specimens, the resin-dentin hybrid layer of approximately 3.5mm thickness was formed and the collapsed collagen layer was observed on the uppermost part of hybrid layer in the specimens applied with All Bond 2. The collgen fibrils of intertubular dentin in specimens applied with Scotchbond Multipurpose were running perpendicular to the interface, and electron dense black layer demarcated from the deep unaltered dentin was more evident in the specimen applied with Superbond D-Liner than any other specimens. 4. In the 1.7 % NaOCl retreated specimens after acid conditioning, the resin-dentin hybrid layer of approximately 2.5-3.0mm thickness was formed and the collapsed collagen layer and longitudinally running collagen fibrils as shown in the acid conditioned specimens were observed in the specimens applied with All Bond 2 and Superbond D-Liner. 5. In all of the 3.3% NaOCl retreated specimens after acid conditioning, the evidence of resin-dentin hybrid layer was not identified ; nevertheless, the longitudinally running collagen fibrils remained slightly in the specimens applied with All Bond 2.

• Restorative Dentistry and Endodontics
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• v.22 no.1
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• pp.209-219
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• 1997

The research of the dentin bonding system was mainly on the chemistry and bonding strength. And in vitro assessement of biocompatibility of dentin bonding system was not completely developed. The purpose of this study was to evaluate the cytotoxic effect of several dentin primers. Scotchbond Multi-Purpose (3M Dental Products. USA). Gluma (BayerDental. Germany). All-Bond (Bisco. USA). ProBond (CaulkDensply, USA) and VeridonFil (Dongyang Nylon. Korea) were included. Cytotoxicity was tested using MTT cell viability test. 0.5 ul. 1 ul. 2 ul and 10 ul of each primer were added to the 96 well plate of incubated L929 cell lines. After 30-minute. 1. 4. 24 and 72-hour exposures. absorbance of L929 cells was observed with ELISA reader. All data were analyzed using t-test. All primers showed cytotoxicity on L929 cells under every conditions used in this study. Absorbance of L929 cells was decreased by time. Scotch bond group exhibited the lowest absorbance value in all exposure time and value.

• The Journal of Advanced Prosthodontics
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• v.6 no.6
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• pp.451-455
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• 2014

PURPOSE. The most common failure seen in restorations with a zirconia core is total or layered delamination of the ceramic veneer. In the present study, the shear bond strengths between veneering ceramics and colored zirconia oxide core materials were evaluated. MATERIALS AND METHODS. Zirconia discs ($15{\times}12{\times}1.6mm$) were divided into 11 groups of 12 discs each. Groups were colored according to the Vita Classic scale: A3, B1, C4, D2, and D4. Each group was treated with the recommended shading time for 3 s, or with prolonged shading for 60 s, except for the control group. Samples were veneered with 3 mm thick and 3.5 mm in diameter translucent ceramic and subjected to shear test in a universal testing machine with a crosshead speed of 1 mm/min. One-way analysis of variance (ANOVA) and Tukey's HSD tests were used for comparisons of the groups having the same shading times. A paired t-test was used for groups of the same color (3 s/60 s). RESULTS. Among the 11 groups investigated C4 (3 s) had the highest bond strength with a value of 36.40 MPa, while A3 (3 s) showed the lowest bond strength with a value of 29.47 MPa. CONCLUSION. Coloring procedures can affect zirconia/ceramic bond strength. However, the results also showed that bond strengths of all the investigated groups were clinically acceptable.

• The Journal of Korean Academy of Prosthodontics
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• v.35 no.3
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• pp.458-469
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• 1997

This study was to compare the tensile bond strength and flexibility of four different soft liners(Coe-Soft, Soft Relining, Soft-Liner, Dura Base Soft) before & after thermocycling. Each soft liner was bonded to denture base resin block, and measured the tensile bond strength and modulus of elasticity using Universal testing machine. The mean value of tensile bond strength and modulus of elasticity for each experimental groups were statistically processed by SPSS(Statistical Package of Social Science). The obtained results were as follows : 1. Dura Base Soft had the highest tensile bond strength and Coe-Soft had the lowest tensile bond strength. 2. Coe-Soft had the lowest modulus of elasticity, and Dura Base Soft had the highest modulus of elasticity. 3. Thermocycling had no effects on the tensile bond strength and modulus of elasticity of all the soft liners. 4. The failure modes of Coe-Soft, Soft Relining, Soft Liner were mainly cohesive failure, and that of Dura Base Soft were mainly adhesive failure.

• The Journal of Korean Academy of Prosthodontics
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• v.40 no.4
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• pp.396-405
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• 2002

The purpose of this study was to evaluate the effects of four metal surface treatments on the shear bond strength of reline resin to Ni-Cr alloy. The denture base metal used in this study was Ni-Cr alloy(Ticonium Premium 100. Ticonium Co., U.S.A.). 120 specimens were divided into five metal surface treatments: sandblasting only, MR. BOND(Tokuyama Corp.. Japan), Cesead Opaque Primer(Kuraray Co., Japan), METALPRIMER II(GC Corp., Japan) and Super-Bond C&B(Sun Medical Co., Japan) after sandblasting. They were bonded with one of three reline resins Mild Rebaron(GC Corp., Japan), Mild Rebaron LC(GC Corp., Japan) and Meta Base M(Sun Medical Co., Japan). Then they were thermocycled 1,000 times at temperature of $4^{\circ}C$ and $60^{\circ}C$. The shear bond strengths were measured using the universal testing machine(Instron, Model 4301, England) with a cross-head speed of 2 mm/min. The results were as follows : 1. All metal primers and adhesive cement significantly improved the bond strength of reline resin to Ni-Cr alloy compared with sandblasted specimens. 2. In Mild Rebaron and Mild Rebaron LC. Cesead Opaque Primer showed the highest bond strength, but the differences among Cesead Opaque Primer, MR. BOND and METALPRIMER II were not significant. The bond strength of Cesead Opaque Primer was significantly different with that of Super-Bond C&B. 3. In Meta Base M, Super-Bond C&B showed the highest bond strength, but there was no difference between Super-Bond C&B and three metal primers. 4. There was no difference in the bond strength between Mild Rebaron and Mild Rebaron LC when metal surface was treated with the same method. 5. The bond strengths of Mild Rebaron and Mild Rebaron LC treated with Cesead Opaque Primer were higher than that of Meta Base M. The bond strengths of Mild Rebaron treated with MR. BOND and METALPRIMER II was higher than that of Meta Base M, However, there was no difference among three reline resins treated with Super-Bond C&B.

• Restorative Dentistry and Endodontics
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• v.21 no.2
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• pp.602-618
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• 1996

The purpose of this study was to investigate the effect of acid treatment of fluoride applied dentin surface with various concentrations of phosphoric acid for various periods of time on dentin bonding. Dentin specimens prepared from freshly extracted bovine mandibular anterior teeth were divided into fluoridated and nonfluoridated groups. Specimens of nonfluoridated group were pretreated with 10% phosphoric acid for 15 seconds. Those of fluoridated groups were treated with 2% sodium fluoride or 2% stannous fluoride solution for 5 minutes and stored in $37^{\circ}C$ distilled water for 3 days, followed by phosphoric acid treatment. The concentrations of phosphoric acid were 10%, 32% or 50% and the treatment periods of time were 15, 30 or 60 seconds. All the specimens were bonded with All Bond$^{(R)}$ 2 and Bisfil$^{TM}$ composite resin. After bonded specimens were stored in $37^{\circ}C$ distilled water for 24 hours, tensile bond strengths of each specimens were measured and the pretreated dentin and the fractured dentin surfaces were examined under the scanning electron microscope. The results were as follows : The tensile bond strengths from the fluoridated groups were significantly lower than those from the nonfluoridated group when the concentrations of phosphoric acid and the treatment periods of time were equal in all the groups (p<0.05). In general, the higher the concentration of phosphoric acid and the longer the treatment period of time for acid etching on the fluoride applied dentin surface, the higher were the bond strength values. Recovery of bond strength of the dentin bonding agent was better in the NaF applied group than in the $SnF_2$ applied one. SEM findings of NaF applied and $SnF_2$ applied dentin surfaces demonstrated reaction product-covered and partially or completely obstructed dentinal tubules. SEM findings of dentin surfaces fluoridated for 5 minutes followed by etching showed wider tubular openings and more clean dentin surfaces when dentin was etched with higher concentration of phosphoric acid for longer period of time. On the SEM observations of the fractured dentin-resin interface, the etched specimens of fluoridated group showed an adhesive failure mode when the concentration of phosphoric acid and the treatment period of time were same as in the nonfluoridated group. As the concentration of phosphoric acid and the treatment period of time increase during acid etching, the cohesive failure area increased. However, excessive acid etching caused adhesive failure.

• Restorative Dentistry and Endodontics
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• v.20 no.1
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• pp.1-16
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• 1995

The purpose of this study was to investigate the effect of dentin bonding agents on the bond strength of composite resin restorations in case of applying the dentin bonding agents to acid etched enamel surfaces. Freshly extracted 364 bovine anterior teeth were selected as a adherents. 320 enamel specimens were divided into two groups(unetched group (1) and etched group (2) for testing the shear bond strength, 40 specimens were used for the hardness testing, and 4 specimens of rest were to observe the resin-tag formation into etched enamel surfaces. All surfaces of enamel specimens were polished with 320~1500 SiC paper under continuous running water. In Group (1), 100 enamel specimens were polished and unetched. 220 polished enamel specimens in Group (2) were etched with 37 % phosphoric acid solution for 60 seconds, washed with water for 20 seconds, and dried with a light air pressure for 60 seconds. Three kinds of dentin bonding agents(Gluma, Prisma, Scotchbond 2) were evaluated the effect on the bond strength to conditioned enamel surfaces. Shear bond strengths were measured on the three cases such as a coating of primer only, a coating of sealer only, and a sequential coating of primer and sealer to acid etched enamel surfaces were compared with the bond strengths measured by the coating of enamel bonding agent followed by the bonding of composite resin (Photo clearfil bright, Kuraray, Japan) to unetched and acid etched enamel surfaces. In addition, the hardness tested on the adhesive fractured surface between composite resin enamel as a mean of evaluation of a factor whether the mechanical bond strengths were affected and the penetration of dentin bonding agents into etched enamel surfaces was also observed. Bond strengths were measured using the method of shear bond strength by a universal testing machine (Instron-4467, USA), statistical test were applied to the results using a one way analysis variance(ANOVA), and hardness was measured by the Vicker's Hardness Tester(MHT-i, Matsuzawa, Japan) and the penetration of the resins were observed by the SEM (Hitachi, S-2300, Japan). The following conclusions were drawn; 1. Enamel bonding agent showed to affect the improvement of bond strength of composite resin to enamel surface both unetched and etched. 2. Dentin bonding agents could be resulted in increase of bond strength to unetched enamel surface, but there were no statistical significances. 3. Bond strengths to etched enamel surface were significantly decreased with a coating of dentin primer only. 4. Coating of sealer only and coating of primer and sealer noticed the similar bond strengths of composite resin to etched enamel using the enamel bonding agents. 5. The applying method proved to be more effective than the kinds of dentin bonding agents on the bond strength of composite resin to etched enamel than the kind of dentin. 6. Vicker's hardness numbers of dentin bonding agents were lower than that of composite resin, but the degree of penetration of dentin bonding agents into etched enamel surfaces was excellent.

• Journal of the korean academy of Pediatric Dentistry
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• v.27 no.3
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• pp.444-456
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• 2000

To test the shear bond strength of a new "one-bottle adhesive" system to primary dentin two commercially available one-bottle adhesives (Prime & Bond NT, Single bond) and conventional three step system(Scotchbond Multi-Purpose Plus) were included for comparison. And We observe the interfacial morphology by scanning electron microscope. 90 primary molar teeth were embedded in acrylic and buccal and lingual surface were polished to 320 grit to create standardized dentin surface for testing. After bonding of composite resin to sample surfaces according to the manufacturer s direction and 1000 times thermocycling in dwell time 30 second, Shear bond strengths of adhesives to dentin were determined using universal testing machine and analyzed by ANOVA test. Another groups of specimens were treated by hydrochloric acid to secure the resin only and those tags were evaluated under SEM for their length and forms and the morphology of the bonding sites were also observed. The result are as follows. 1. Group I(Prime & Bond NT) showed higher shear bond strength than group iI(Single Bond) and III(Scotchbond Multi Purpose Plus) but no statistically significant difference was founded between groups(p>.05). 2. Relating long resin tags of $70-120{\mu}m$ were observed in samples of all groups under SEM. We could observed hybrid layer, resin tag and many lateral branches in every group. But, we observed in group III rare lateral branched than other two group and discontinuous hybrid layer.

• Restorative Dentistry and Endodontics
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• v.20 no.1
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• pp.214-234
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• 1995

The purpose of this work was to study the compatibility of several commercially available dentin adhesives with composite resins. In this study, V-shaped cavity preparations were created on both buccal and lingual surfaces of 60 extracted human premolars($3mm{\times}3mm{\times}2mm$ deep). Preparations were located such that the occlusal margins were on the enamel and the gingival margins were on the cementum(1mm below the CEJ). These specimens were randomly divided into three equal groups. Three dentin adhesives(Scotchbond Multi-Purpose, All Bond 2, Prisma Universal Bond 3)were applied to the cavity in accordance with each manufacturer's instructions. The teeth in each group were restored with four composite resins(Silux plus, Z100, Bisfil, Prisma TPH) in three increments, with each increment light-cured for 40 seconds. All specimens were exposed to 500 cycles of thermal stress. Specimens then placed in a silver nitrate solution(50% by weight) and stored in darkness for 24 hours. They were then immersed for 6 hours in photographic developing solution under flourescent light. Specimens were sectioned buccolingually through the center of the restoration and observed under a binocular stereoscope. To compare the marginal leakage, ANOVA and Dunkan's multiple range tests were used in analysis. Selected samples were further studied using scanning electron microscopy(XL20, Philips, The Netherlands). The results were as follows. 1. In all groups, the enamel margin showed significantly less leakage than the cementum margin. 2. No statistically significant differences were found in microleakage when composite resins were used with their proprietary dentin adhesives. 3. In comparison between dentin adhesives, Prisma Universal Bond 3 showed significantly less leakage at the enamel margin and Scotch bond multi-purpose showed significantly less leakage at the cementum margin than the other groups. 4. In comparison between composite resins, Silux Plus showed significantly more leakage than other groups at the enamel margin and no statistically significant differences were found in microleakage at the cementum margin. 5. According to the backscattered scanning electron microscope, microleakage occurred via gaps at the dentin adhesives/dentin interface.