• The Journal of Advanced Prosthodontics
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• v.9 no.2
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• pp.85-92
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• 2017

PURPOSE. The aim of this study was to evaluate the effect of tooth surface pre-treatment steps on shear bond strength, which is essential for understanding the adhesive cementation process. MATERIALS AND METHODS. Shear bond strengths of different cements with various tooth surface treatments (none, etching, priming, or etching and priming) on enamel and dentin of human teeth were measured using the Swiss shear test design. Three adhesives (Permaflo DC, Panavia F 2.0, and Panavia V5) and one self-adhesive cement (Panavia SA plus) were included in this study. The interface of the cement and the tooth surface with the different pre-treatments was analyzed using SEM. pH values of the cements and primers were measured. RESULTS. The highest bond strength values for all cements were achieved with etching and primer on enamel ($25.6{\pm}5.3-32.3{\pm}10.4MPa$). On dentin, etching and priming produced the highest bond strength values for all cements ($8.6{\pm}2.9-11.7{\pm}3.5MPa$) except for Panavia V5, which achieved significantly higher bond strengths when pre-treated with primer only ($15.3{\pm}4.1MPa$). Shear bond strength values were correlated with the micro-retentive surface topography of enamel and the tag length on dentin except for Panavia V5, which revealed the highest bond strength with primer application only without etching, resulting in short but sturdy tags. CONCLUSION. The highest bond strength can be achieved for Panavia F 2.0, Permaflo DC, and Panavia SA plus when the tooth substrate is previously etched and the respective primer is applied. The new cement Panavia V5 displayed low technique-sensitivity and attained significantly higher adhesion of all tested cements to dentin when only primer was applied.

• Restorative Dentistry and Endodontics
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• v.12 no.2
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• pp.101-108
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• 1987

The purpose of this study was to investigate the pulpal responses of dental adhesive resins. A total of 40 cavities of the permanent healthy teeth from 4 dogs were prepared. In the experimental group, the cavities were etched for 1 minute with citric acid and filled with experimental resins (ie. Super-Bond C & B$^{(R)}$). In the control group, the cavities were filled with calcium hydroxide base materials (ie. Dycal$^{(R)}$) without etching. The dogs were sacrificed at one, two, three and four weeks after the time of filling and the specimens were routinely prepared and stained with Hematoxylin-Eosin. The microscopic findings were as follows: Infiltration of inflammatory cells was not observed in both experimental and control groups. Change in the odontoblastic layer was not observed in all control groups but severe swelling was observed in deep dental pulp tissue of the control two and three week cases. Pulp tissue was recovered with plenty of fibrous component in the control four week case and reparative dentin formation was not occurred in all cases. Slight changes of the odontoblastic layer beneath the cavity were observed in the experimental one week case. In experimental two and three week cases, swelling of deep pulp tissue was increased and localized reparative dentin formation was observed. In the experimental four week case, odontoblastic layer was recovered with regular appearance and fibrous component of the pulp was increased, but reparative dentin formation was not evident.

• The Journal of Korean Academy of Prosthodontics
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• v.46 no.5
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• pp.535-543
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• 2008

Purpose: The objective of this study was to compare the bonding characteristics of a new self-adhesive resin cement to dentin, which does not require bonding and conditioning procedure of the tooth surface, and conventional resin cement. The effect of phosphoric acid etching prior to application of self-adhesive resin cement on the shear bond strength was also evaluated. Material and methods: Fortyfive non-carious human adult molars extracted within 6 months were embedded in chemically cured acrylic resin. The teeth were ground with a series of SiC-papers ending with 800 grit until the flat dentin surfaces of the teeth were exposed. The teeth were randomly divided into 3 experimental groups. In group 1, self-adhesive resin cement, RelyX Unicem (3M ESPE, Seefeld, Germany) was bonded without any conditioning of teeth. In group 2, RelyX Unicem was bonded to teeth after phosphoric acid etching. For group 3, Syntac Primer (Ivoclar Vivadent AG, Schaan, Liechtenstein) was applied to the teeth before Syntac adhesive (Ivoclar Vivadent AG, Schaan, Liechtenstein) and Helibond (Ivoclar Vivadent AG, Schaan, Liechtenstein) followed by conventional resin cement, Variolink II (Ivoclar Vivadent AG, Schaan, Liechtenstein). To make a shear bond strength test model, a plastic tuble (3 mm diameter, 3 mm height) was applied to the dentin surfaces at a right angle and filled it with respective resin cement, and light-polymerized for 40 seconds. All the specimens were stored in distilled water at $37^{\circ}C$ for 24 hours before test. Universal Testing Machine (Z020, Zwick, Ulm, Germany) at a cross head speed of 1 mm/min was used to evaluate the shear bond strength. The failure sites were inspected under a magnifier and Scanning Electron Microscope. The data was analyzed with One way ANOVA and Scheffe test at ${\alpha}$= 0.05. Results: (1) The shear bond strengths to dentin of RelyX Unicem was not significantly different from those of Variolink II/Syntac. (2) Phosphoric acid etching lowered the shear bond strength of RelyX Unicem significantly. (3) Most of RelyX Unicem and Variolink II showed mixed fractures, while all the specimens of RelyX Unicem with phosphoric acid etching demonstrated adhesive failure between dentin and resin cement. Conclusion: Shear bond strength to dentin of self-adhesive resin cement is not significantly different from conventional resin cement, and phosphoric acid etching decrease the shear bond strength to dentin of self-adhesive resin cement.

• Restorative Dentistry and Endodontics
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• v.24 no.1
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• pp.240-250
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• 1999

The purpose of this study was to evaluate the effect of different etching time on the shear bond strength and adaptibility of composite to enamel and dentin when used one-bottle adhesive Prime & Bond$^{TM}$ 2.0. The proximal and occlusal surfaces of 88 extracted human molars were ground to expose enamel(n=44) and dentin (=44) using diamond wheel saw. Teeth were randomly assigned to four test groups(n=11) and received the following treatments : Control group were conditioned with 36% phosphoric acid for 20 sec. according to the manufacturer's directions. Experimental 10 sec. group, 30 sec. group and 60 sec. group were conditioned with 36% phosphoric acid for 10 sec., 30 sec. and 60 sec., respectively. Teeth were rinsed and dried for 2 sec. Prime & Bond$^{TM}$ 2.0 were applied according to the manufacturer's directions and Spectrum$^{TM}$ TPH composite resins were bonded to enamel and dentin surfaces. All specimens were stored in distilled water for 24 hours. Eighty specimens were sheared in a Universal Testing Machine with a crosshead speed of 5mm/minute. One way ANOVA and LSD test were used for statistical analysis of the data. Failure modes of all specimens after shear bond strength test were examined and listed. Also, representive postfracture modes and eight specimens were examined under scanning electron microscope. The results of this study were as follows: 1. The shear bond strength to enamel was the highest value in 30 sec. group (20.68${\pm}$8.54MPa) and the lowest value in 10 sec. group (14.92${\pm}$6.07MPa), so there was significant difference of shear bond strength between two groups (p<0.05). But there was no significant difference among other groups (p>0.05). With longer etching time to enamel from 10 sec. to 30 sec., higher the shear bond strength was obtained, but the shear bond strength was decreased at 60 sec. etching time. 2. The shear bond strength to dentin was the highest value in control group (13.08${\pm}$6.25MPa) and the lowest value in 60 sec. group (9.47${\pm}$3.35MPa), but there was no significant difference among the all groups (p>0.05). The eching time over 20 sec. decreased the shear bond strength to dentin. 3. In SEM observation, the enamel and resin interfaces were showed close adaptation with no relation to etching time of enamel. And the dentin and resin interfaces were showed close adaptation at 20 sec. and 30 sec. etching time, but showed some gaps at 10 sec. and 60 sec. etching time. Accordingly, these results indicated that a appropriate etching time in Prime & Bond$^{TM}$ 2.0 was required to be 30 sec. in enamel and 20 sec. in dentin for the high shear bond strength and good adaptation between the composite resin and tooth substance.

• Restorative Dentistry and Endodontics
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• v.21 no.1
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• pp.321-338
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• 1996

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.

• 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.35 no.2
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• pp.106-115
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• 2010

The purpose of this study was to evaluate the microtensile bond strength (${\mu}TBS$), failure modes and bonding interfaces of self-etching and three self-adhesive resin cements to dentin and indirect composite resin. Cylindrical composite blocks (Tescera, Bisco Inc.) were luted with resin cements (PA: Panavia F 2.0, Kuraray Medical Inc., RE: RelyX Unicem Clicker, 3M ESPE., MA: Maxem, Kerr Co., BI: BisCem, Bisco Inc.) on the prepared occlusal dentin surfaces of 20 extracted molars. After storage in distilled water for 24 h, $1.0\;mm\;{\times}\;1.0\;mm$ composite-dentin beams were prepared. ${\mu}TBS$ was tested at a cross-head speed of 0.5 mm/min. Data were analyzed with one-way ANOVA and Tukey's HSD test. Dentin sides of all fractured specimens and interfaces of resin cements-dentin or resin cements-composite were examined at FESEM (Field Emission-Scanning Electron Microscope). In conclusion, PA and RE showed higher bond strength and closer adaptation than MA and BI when indirect composite blocks were luted to dentin using a self-etching and three self-adhesive resin cements.

• Journal of Korean Dental Science
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• v.2 no.2
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• pp.5-11
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• 2009

Objectives : This study investigated the hypothesis that the dentin bond strength of self-etching adhesives (SEAs) may be improved by applying a coat of hydrophobic, neutral adhesive resin in addition to SEA. Method and Materials : The bond strengths of two SEAs - Experimental SEA (EX) and Adper Prompt (AP) - were measured with three bonding protocols. The D/E resin of All-Bond 2 was applied as the hydrophobic, neutral adhesive. Clearfil SE Bond (SE, self-etching primer system) and All-Bond 2 (AB, total etching system) were used as references. The following protocols were used: (1) EX1 (EX 1 coat); (2) EX2 (EX 2 coats); (3) EX+ (EX 1 coat + D/E resin); (4) AP1 (AP 1 coat); (5) AP2 (AP 2 coats); (6) AP+ (AP 1 coat + D/E resin); (7) SE (SE primer + SE bond); (8) SE+ (SE primer + D/E resin); (9) AB (etching + AB primer + D/E resin). Filtek Z250 composite resin was built up and the microtensile bond strength (MTBS) values of the specimens were compared. The fractured surfaces were observed using SEM. Results : When SEA was used as self-etching primer and hydrophobic, neutral adhesive was applied as well, MTBS was significantly higher than that when either one coat or two coats of SEA only were used (p < 0.05). Conclusion : The hydrophobic, neutral adhesive improved the integrity of the bonded interface obtained with SEA.

• Restorative Dentistry and Endodontics
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• v.46 no.2
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• pp.30.1-30.13
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• 2021

Objectives: This study was conducted to compare the microleakage and characteristics of the resin-tooth tissue interface between self-etch and etch-and-rinse adhesive systems after 48 hours and 3 months. Materials and Methods: 40 extracted premolar teeth were randomly divided into 2 groups: 1-step self-etch adhesive system - Optibond^TM All-In-One, and 2-step etch-and-rinse adhesive system - Adper^TM Single Bond 2. Both groups were subjected to 500 thermocycles (5℃-55℃) before scanning electron microscope (SEM) analysis or microleakage trial at 48-hour and 3-month time periods. Results: SEM images showed the hybrid layer thickness, diameter, and length of resin tags of the self-etch adhesive (0.42 ± 0.14 ㎛; 1.49 ± 0.45 ㎛; 16.35 ± 14.26 ㎛) were smaller than those of the etch-and-rinse adhesive (4.39 ± 1.52 ㎛; 3.49 ± 1 ㎛; 52.81 ± 35.81 ㎛). In dentin, the microleakage scores of the 2 adhesives were not different in both time periods (48 hours/3 months). However, the microleakage score of etch-and-rinse adhesive increased significantly after 3 months (0.8 ± 0.63 and 1.9 ± 0.88, p < 0.05). Conclusions: The self-etch adhesive exhibited better long-term sealing ability in dentin when compared to that of the etch-and-rinse adhesive. The greater hybrid layer thickness and dimensions of resin tags did not guarantee reliable, long-lasting sealing in the bonding area.

• Restorative Dentistry and Endodontics
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• v.24 no.4
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• pp.647-656
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• 1999

The purpose of this study was to investigate the shear bond strength and marginal microleakage of composite to enamel and dentin according to different treatment methods when the applied bonding agent was contaminated by artificial saliva. For the shear bond strength test, the buccal and occlusal surfaces of one hundred twenty molar teeth were ground to expose enamel(n=60) and dentin surfaces(n=60). The specimens were randomly assigned into control and 5 experimental groups with 10 samples in each group. In control group, a bonding system(Scotchbond$^{TM}$ Multi-Purpose plus) and a composite resin(Z-100$^{TM}$) was bonded on the specimens according to manufacture's directions. Experimental groups were subdivided into 5 groups. After polymerization of an adhesive, they were contaminated with at artificial saliva on enamel and dentin surfaces: Experimental group 1 ; artificial saliva was dried with compressed air. Experimental group 2 ; artificial saliva was rinsed with air-water spray and dried. Experimental group 3 ; artificial saliva was rinsed, dried and applied an adhesive. Experimental group 4 ; artificial saliva was rinsed, dried, and then etched using phosphoric acid followed by an adhesive. Experimental group 5, artificial saliva was rinsed, dried, and then etched with phosphoric acid followed by consecutive application of both a primer and an adhesive. Composite resin(Z-100$^{TM}$) was bonded on saliva-treated enamel and dentin surfaces. The shear bond strengths were measured by universal testing machine(AGS-1000 4D, Shimaduzu Co. Japan) with a crosshead speed of 5mm/minute under 50kg load cell. Failure modes of fracture sites were examined under stereomicroscope. The data were analyzed by one-way ANOVA and Tukey's test. For the marginal microleakage test, Class V cavities were prepared on the buccal surfaces of sixty molars. The specimens were divided into control and experimental groups. Cavities in experimental group were contaminated with artificial saliva and those surfaces in each experimental groups received the same treatments as for the shear test. Cavities were filled with Z-100. Specimens were immersed in 0.5% basic fuchsin dye for 24 hours and embedded in transparent acrylic resin and sectioned buccolingually with diamond wheel saw. Four sections were obtained from the one specimen. Marginal microleakages of enamel and dentin were scored under streomicroscope and averaged from four sections. The data were analyzed by Kruskal-Wallis test and Fisher's LSD. The results of this study were as follows. 1. The shear bond strength to enamel showed lower value in experimental group 1(13.20${\pm}$2.94MPa) and experimental group 2(13.20${\pm}$2.94MPa) than in control(20.03${\pm}$4.47MPa), experimental group 4(20.96${\pm}$4.25MPa) and experimental group 5(21.25${\pm}$4.48MPa) (p<0.05). 2. The shear bond strength to dentin showed lower value in experimental group 1(9.35${\pm}$4.11MPa) and experimental group 2(9.83${\pm}$4.11MPa) than in control group(17.86${\pm}$4.03MPa), experimental group 4(15.04${\pm}$3.22MPa) and experimental group 5(14.33${\pm}$3.00MPa) (p<0.05). 3. Both on enamel and dentin surfaces, experimental group 1 and 2 showed many adhesive failures, but control and experimental group 3, 4 and 5 showed mixed and cohesive failures. 4. Enamel marginal microleakage was the highest in experimental group 1 and there was a significant difference in comparison with other groups (p<0.05). 5. Dentin marginal microleakages of experimental group 1 and 2 were higher than those of other groups (p<0.05). This result suggests that treatment methods, re-etching with 35% phosphoric acid followed by re-application of adhesive or repeating all adhesive procedures, will produce good effect on both shear bond strength and microleakage of composite to enamel and dentin if the polymerized bonding agent was contaminated by saliva.