• Restorative Dentistry and Endodontics
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• v.36 no.2
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• pp.139-148
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• 2011

Objectives: This study investigated the effect of the strength and wetting characteristics of adhesives on the bond strength to dentin. The experimental adhesives containing various ratios of hydrophobic, low-viscosity Bis-M-GMA, with Bis-GMA and TEGDMA, were made and evaluated on the mechanical properties and bond strength to dentin. Materials and Methods: Five experimental adhesives formulated with various Bis-GMA/Bis-MGMA/TEGDMA ratios were evaluated on their viscosity, degree of conversion (DC), flexural strength (FS), and microtensile bond strength (MTBS). The bonded interfaces were evaluated with SEM and the solubility parameter was calculated to understand the wetting characteristics of the adhesives. Results: Although there were no significant differences in the DC between the experimental adhesives at 48 hr after curing (p > 0.05), the experimental adhesives that did not contain Bis-GMA exhibited a lower FS than did those containing Bis-GMA (p < 0.05). The experimental adhesives that had very little to no TEGDMA showed significantly lower MTBS than did those containing a higher content of TEGDMA (p < 0.05). The formers exhibited gaps at the interface between the adhesive layer and the hybrid layer. The solubility parameter of TEGDMA approximated those of the components of the primed dentin, rather than Bis-GMA and Bis-M-GMA. Conclusions: To achieve a good dentin bond, a strong base monomer, such as Bis-GMA, cannot be completely replaced by Bis-M-GMA for maintaining mechanical strength. For compatible copolymerization between the adhesive and the primed dentin as well as dense cross-linking of the adhesive layer, at least 30% fraction of TEGDMA is also needed.

• Restorative Dentistry and Endodontics
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• v.33 no.1
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• pp.9-19
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• 2008

The purpose of this study was: (1) to compare nanoleakage patterns of a conventional 3-step etch and rinse adhesive system and two experimental hydrophobic adhesive systems and (2) to investigate the change of the nanoleakage patterns after load cycling. Two kinds of hydrophobic experimental adhesives, ethanol containing adhesive (EA) and methanol containing adhesive (MA), were prepared. Thirty extracted human molars were embedded in resin blocks and occlusal thirds of the crowns were removed. The polished dentin surfaces were etched with a 35 % phosphoric acid etching gel and rinsed with water. Scotchbond Multi-Purpose (MP), EA and MA were used for bonding procedure. Z-250 composite resin was built-up on the adhesive-treated surfaces. Five teeth of each dentin adhesive group were subjected to mechanical load cycling. The teeth were sectioned into 2 mm thick slabs and then stained with 50 % ammoniacal silver nitrate. Ten specimens for each group were examined under scanning electron microscope in backscattering electron mode. All photographs were analyzed using image analysis software. Three regions of each specimen were used for evaluation of the silver uptake within the hybrid layer. The area of silver deposition was calculated and expressed in gray value. Data were statistically analyzed by two-way ANOVA and post-hoc testing of multiple comparisons was done with the Scheffe's test. Silver particles were observed in all the groups. However, silver particles were more sparsely distributed in the EA group and the MA group than in the MP group (p < .0001). There were no changes in nanoleakage patterns after load cycling.

• Journal of Dental Rehabilitation and Applied Science
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• v.24 no.1
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• pp.105-112
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• 2008

The purpose of this study was to evaluate the contact angle made by 3 kinds of self etching primers (Clearfil SE Bond, AdheSE, and Tyrian) on dentin and to measure the microtensile bond strength of resin composite to dentin using these self-etching primers. Contact angle between each of 3 self etching primers and polished dentin surface was measured (n=30) by contact angle analyzer and the result was analyzed by One-way ANOVA. For the measurement of microtensile bond strength, polished dentin surface was treated with each of 3 self etching primers and dentin adhesives. Z-250 composite resin was built-up with a height of 5 mm on the adhesive-treated surface and light cured for 40s with a halogen light curing unit. Thereafter, each tooth was sectioned into slabs perpendicular to the bonded interface and trimmed (n=45). The microtensile bond strength was measured with universal testing machine and the result was analyzed with Kruskal-Wallis test. AdheSE group showed the highest contact angle followed by Clearfil SE group and Tyrian group (p<0.05). AdheSE group and Clearfil SE group showed significantly higher microtensile bond strength than Tyrian group (P<0.05).

• Restorative Dentistry and Endodontics
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• v.24 no.4
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• pp.570-577
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• 1999

Intuitively, higher bond strengths should result in less leakage. However, the relationship between bond strengths and microleakage value is complex and not clearly understood. The purpose of this study was to evaluate the relationship between tensile bond strengths and microleakage values in the same restorations to understand the behavior of resin bonding to tooth structure. One-hundred and twenty enamel or dentin specimens from freshly extracted bovine mandibular incisors were used. The specimen was treated with 32% phosphoric acid for 15 seconds and rinsed for 20 seconds. the teeth were divided into four groups by means of wet bonding technique or dry bonding. One-Step$^{TM}$ adhesive were applied to the specimen. The specimens were immersed in 2% methylene blue solution for 7 days, and tensile bond strength and microleakage were measured. The results were as follows: 1. Significant negative correlation was found between bond strengths and micro leakage values. Hence, higher bond strengths seem to be associated with lower microleakage, and vice versa (r=-0 50, p<0.05). 2. The Enamel/Wet group showed significantly higher bond strength than Enamel/Dry one, and Dentin/Wet group showed higher strength than Dentin/Dry one (p<0.05). 3. Microleakage was significantly less ill wet bonding than in dry one at dentin (p<0.05), however, there was no significant difference between wet and dry bonding at enamel (p>0.05).

• Journal of the korean academy of Pediatric Dentistry
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• v.35 no.3
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• pp.389-398
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• 2008

The purpose of this study was to evaluate the effects of collagenase and esterase on dentin bond strength and nanoleakage. Resin composites were bonded to occlusal dentin of premolars with Single Bond 2(SB) and Clearfil SE Bond(SE). After the microtensile specimens were prepared and stored in PBS for 24 hours(I) or, PBS(II), collagenase(III), esterase(IV) solution for 4 weeks, the specimens were stained with silver nitrate solution. Microtensile bond strength(${\mu}TBS$) and silver penetration area were measured and, the results were as follows: 1. For group II, III, and IV, the bond strengths of SB were lower than those of SB(p<0.05). The bond strengths of SB II, III, and IV were lower than that of SB I(p<0.05). There was no difference among the bond strengths of SE $I{\sim}IV$ groups(p>0.05). 2. Silver penetration areas of SB were higher than those of SE for all storage groups(p<0.05). In SB and SE groups, there was no significant difference of silver penetration area among $I{\sim}IV$ groups(p>0.05). 3. SE I, II, and III showed inverse relationship between the bond strengths and the silver penetration areas(p<0.05).

• Restorative Dentistry and Endodontics
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• v.35 no.5
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• pp.321-334
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• 2010

Objectives: The purpose of this study is to evaluate bonding efficacy by means of measuring the effect of remained solvent on Degree of conversion(DC) and ${\mu}TBS$ and FE-SEM examination. Materials and Methods: Two 2-step total etching adhesives and two single-step self etching adhesives were used in this study. First, volume weight loss of 4 dentin adhesives were measured using weighting machine in process of time in normal conditions and calculate degree of evaporation (DE). Reaction/reference intensity ratio were measured using micro-Raman spectroscopy and calculate DC according to DE. Then 2 experimental groups were prepared according to air-drying methods (under, over) and control group was prepared to manufacturer's instruction. Total 12 groups were evaluated by means of micro tensile bond strength and FE-SEM examination. Results: Degree of evaporation (DE) was increased as time elapsed but different features were observed according to the kind of solvents. Acetone based adhesive showed higher DE than ethanol and butanol based adhesive. Degree of conversion (DC) was increased according to DE except for $S^3$ bond. In ${\mu}TBS$ evaluation, bond strength was increased by additional air-drying. Large gaps and droplets were observed in acetone based adhesives by FE-SEM pictures. Conclusions: Additional air-drying is recommended for single-step self etching adhesive but careful consideration is required for 2-step total etching adhesive because of oxygen inhibition layer. Evaporation method is carefully chose and applied according to the solvent type.

• Restorative Dentistry and Endodontics
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• v.35 no.3
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• pp.211-221
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• 2010

Proteoglycan is highly hydrophilic and negatively charged which enable them attract the water. The objective of study was to investigate the effects of Proteoglycan on microtensile bond strength of dentin adhesives and on architecture of dentin collagen matrix of acid etched dentin by removing the chondroitin sulphate attached on Proteoglycan. A flat dentin surface in mid-coronal portion of tooth was prepared. After acid etching, half of the specimens were immersed in 0.1 U/mL chondroitinase ABC (C-ABC) for 48 h at $37^{\circ}C$, while the other half were stored in distilled water. Specimens were bonded with the dentin adhesive using three different bonding techniques (wet, dry and re-wet) followed by microtensile bond strength test. SEM examination was done with debonded specimen, resin-dentin interface and acid-etched dentin surface with/without C-ABC treatment. For the subgroups using wet-bonding or dry-bonding technique, microtensile bond strength showed no significant difference after C-ABC treatment (p > 0.05). Nevertheless, the subgroup using rewetting technique after air dry in the Single Bond 2 group demonstrated a significant decrease of microtensile bond strength after C-ABC treatment. Collagen architecture is loosely packed and some fibrils are aggregated together and relatively collapsed compared with normal acid-etched wet dentin after C-ABC treatment. Further studies are necessary for the contribution to the collagen architecture of noncollagenous protein under the various clinical situations and several dentin conditioners and are also needed about long-term effect on bond strength of dentin adhesive.

• Restorative Dentistry and Endodontics
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• v.32 no.3
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• pp.208-221
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• 2007

The fracture toughness test is believed as a clinically relevant method for assessing the fracture resistance of the dentinal restoratives. The objectives of this study were to measure the fracture toughness $(K_{1C})$ and microtensile bond strength of dentin-resin composite interface and compare their relationship for their use in evaluation of the integrity of the dentin-resin bond. A minimum of six short-rod specimens for fracture toughness test and fifteen specimens for microtensile bond strength test was fabricated for each group of materials used. After all specimens storing for 24 hours in distilled water at $37^{\circ}C$, they were tensile-loaded with an EZ tester universal testing machin. Statistical analysis was performed using ANOVA and Tukey's test at the 95% confidence level, Pearson's coefficient was used to verify the correlation between the mean of fracture toughness and microtensile bond strength. FE-SEM was employed on fractured surface to describe the crack propagation. Fracture toughness value of Clearfil SE Bond (SE) was the highest, followed by Adper Single Bond 2 (SB), OptiBond Solo (OB), ONE-STEP PLUS (0S), ScotchBond Multi-purpose (SM) and there was significant difference between SE and other 4 groups (p < 0.05). There were, however, no significant difference among SB, OB, OS, SM (p > 0.05). Microtensile bond strength of SE was the highest, followed by SB, OB, SM, OS and OS only showed significant lower value (p < 0.05). There was no correlation between fracture toughness and microtensile bond strength values. FE-SEM examination revealed that dentin bonding agent showed different film thickness and different failure pattern according to the film thickness. From the limited results of this study, it was noted that there was statistically no correlation between K1C and ${\mu}TBS$. We can conclude that for obtaining the reliability of bond strength test of dentin bonding agent, we must pay more attention to the test procedure and its profound scrutiny.

• Restorative Dentistry and Endodontics
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• v.29 no.1
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• pp.13-22
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• 2004

본 연구는 치수강 상아질 부위 및 상아질 접착제 종류에 따른 결합 강도를 측정하고 이들 사이의 상관관계를 구명하고자 시행되었다 45개의 대구치를 포매 후, 대조군에서는 교합면 법랑질 제거 후 ＃600 SiC paper까지 순차연마하여 상아질을 노출시켰고, 실험군에서는 치수강 개방 후 1시간동안 NaOCl에 보관 후 axial wall과 pulpal floor를 노출시켰다. 노출된 상아질 면에 상아질 접착제를 적용한 후 Z-100을 충전한 다음 40초간 광중합하였다. 사용된 상아질 접착제는 Scotchbond Multi-Purpose와 Single Bond, Clearfil SE Bond였다. $37^{\circ}C$ 증류수에 24시간 보관 후, 저속 diamond saw를 이용하여 0.7mm 두께로 수직절단하고 고속 diamond point(#104)로 단면적 $1{mm}^2$가 되도록 시편을 제작하고, Universal testing machine에서 미세인장 결합강도를 측정하였다. 1. 모든 상아질 접착제의 미세인장강도는 대조군, axial wall군, pulpal floor군 순으로 감소하는 경향을 보였다. 2. 대조군에서 SM과 BB는 SE에 비해 유의성 있게 높은 결합강도를 나타내었다(p<0.05). 3. SM과 SB는 대조군에 비해 axial wall군과 pulpal floor군에서 유의성있게 낮은 결합강도를 보였으나, SE에서는 pulpal floor군만이 유의성 있게 낮은 결합강도를 보였다(p<0.05). 4. Axial wall군과 pulpal floor군에서는 상아질 접착제의 종류에 따른 유의차를 보이지 않았다. 5. 전자현미경 소견에서는 대조군에 비해 axial wall군과 pulpal floor군이 더 부드러운 접착 계면을 나타내었다. 혼성층의 두께는 결합강도의 감소와는 관련이 없었다.

• Journal of the korean academy of Pediatric Dentistry
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• v.34 no.3
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• pp.420-429
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• 2007

The purpose of this study was to compare the micro ensile bond strength to bovine dentin of several adhesives (SM, Scotch $Bond^{TM}$ Multipurpose; SB, $Adper^{TM}$ Single Bond 2; SE, $Clearfil^{(R)}$ SE Bond; AQ, AQ $Bond^{TM}$; TS, $Clearfil^{(R)}$ tri-S Bond). Except SM and SB, they have a simplified one- or two-step application protocols in compare with the dentin adhesives conventional three-step protocols. For the microtensile bond strength test, the labial surfaces of bovine incisors were used. Following exposure of dentin layer, according to their manufacturer's directions, each dentin adhesives were applied and composite resin blocks were constructed. The teeth were sectioned for specimen and tested microtensile bond strength. Also observed the fracture mode of interface. The obtained results were as follows : 1. The microtensile bond strength values ranged from 51.34 to 24.04 MPa on dentin(in decreasing order, SE, SM, SB, AQ and TS). 2. The highest microtensile bond strength was by SE and SM on bovine dentin, and the lowest by AQ and TS. 3. SM, SB and SE showed cohesive failures and adhesive failure but AQ, TS presented almost adhesive failures. In summary, microtensile bond strengths of single-step adhesives (AQ and TS) on bovine dentin were significantly lower than those of multi-step adhesives (SM, SB and SE) (p<0.05).