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THE EFFECT OF PRIMING ETCHED DENTIN WITH SOLVENT ON THE MICROTENSILE BOND STRENGTH OF HYDROPHOBIC DENTIN ADHESIVE

THE EFFECT OF PRIMING ETCHED DENTIN WITH SOLVENT ON THE MICROTENSILE BOND STRENGTH OF HYDROPHOBIC DENTIN ADHESIVE

Article information

Restor Dent Endod. 2009;34(1):42-50
Publication date (electronic) : 2009 January 14
doi : https://doi.org/10.5395/JKACD.2009.34.1.42
1Department of Conservative Dentistry, School of Dentistry, Seoul National University
2Department of Conservative Dentistry, Seoul National University Bundang Hospital
3Dental Research Institute, Seoul National University
4Department of Chemical Engineering, Choongang University
*Corresponding Author: Byeong-Hoon Cho, Department of Conservative Dentistry, School of Dentistry, Dental Research Institute, Seoul National University. 28-2 Yeongun-dong, Chongro-gu, Seoul, Korea 110-749, TEL +82-2-2072-3514 FAX +82-2-764-3514, E-mail: chobh@snu.ac.kr
Received 2008 November 18; Revised 2008 December 22; Accepted 2008 December 31.

Abstract

Abstract

Deterioration of long-term dentin adhesion durability is thought to occur by hydrolytic degradation within hydrophilic domains of the adhesive and hybrid layers. This study investigated the hypothesis that priming the collagen network with an organic solvent displace water without collapse and thereby obtain good bond strength with an adhesive made of hydrophobic monomers and organic solvents. Three experimental adhesives were prepared by dissolving two hydrophobic monomers, bisphenol-A-glycidylmethacrylate (Bis-GMA) and triethylenegly-col dimethacrylate (TEGDMA), into acetone, ethanol or methanol. After an etching and rinsing procedure, the adhesives were applied onto either wet dentin surfaces (wet bonding) or dentin surfaces primed with the same solvent (solvent-primed bonding). Microtensile bond strength (MTBS) was measured at 48 hrs, 1 month and after 10,000 times of thermocycles. The bonded interfaces were evaluated using a scanning electron microscope (SEM). Regardless of bonding protocols, well-developed hybrid layers were observed at the bonded interface in most specimens. The highest mean MTBS was observed in the adhesive containing ethanol at 48 hrs. With solvent-primed bonding, increased MTBS tendencies were seen with thermocycling in the adhesives containing ethanol or methanol. However, in the case of wet bonding, no increase in MTBS was observed with aging.

Figure 1.

Microtensile bond strength (MPa) of three experimental adhesives according to the bonding protocols and measuring times.

Figure 2.

Scanning electron microscopic images of the bonded interfaces. a & b, the adhesive containing acetone was applied on acetone-primed dentin after etching and rinsing procedure; c & d, the adhesive containing acetone was applied with wet bonding protocol; e & f, the adhesive containing ethanol was applied on ethanol-primed dentin after etching and rinsing procedure; g & h, the adhesive containing ethanol was applied with wet bonding protocol; i & j, the adhesive containing methanol was applied on methanol-primed dentin after etching and rinsing procedure; k & l, the adhesive containing methanol was applied with wet bonding protocol. Left column, the micrographs taken directly from the specimens; Right column, those taken from the replica of the specimens.

Figure 3.

Fractured surfaces of the bonded specimens. a, dentin side of fractured specimen bonded with adhesive containing methanol using wet bonding. Most failures occurred between the hybrid layer and the adhesive layer. b, dentin side of fractured specimen bonded with adhesive containing ethanol using solvent-primed bonding. In this group, most of the specimens showed mixed fracture.

Figure 4.

Scanning electron microscopic images of the bonded interfaces after thermocycling. a, the adhesive containing acetone was applied with wet bonding protocol; b, the adhesive containing methanol was applied with wet bonding; c, the adhesive containing methanol was applied on methanol-primed dentin after etching and rinsing procedure. With wet bonding protocol, the interfacial gaps were still observed at the same interface as the specimens observed at 48 hrs. However, with solvent-primed bonding protocol, well-developed hybrid layers and a number of long resin tags were observed without apparent interfacial gap.

Materials used for the preparation of the experimental resin adhesives

Microtensile bond strengths of experimental adhesives with different bonding protocols and measuring times (MTBS, unit: MPa)

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Article information Continued

Figure 1.

Microtensile bond strength (MPa) of three experimental adhesives according to the bonding protocols and measuring times.

Figure 2.

Scanning electron microscopic images of the bonded interfaces. a & b, the adhesive containing acetone was applied on acetone-primed dentin after etching and rinsing procedure; c & d, the adhesive containing acetone was applied with wet bonding protocol; e & f, the adhesive containing ethanol was applied on ethanol-primed dentin after etching and rinsing procedure; g & h, the adhesive containing ethanol was applied with wet bonding protocol; i & j, the adhesive containing methanol was applied on methanol-primed dentin after etching and rinsing procedure; k & l, the adhesive containing methanol was applied with wet bonding protocol. Left column, the micrographs taken directly from the specimens; Right column, those taken from the replica of the specimens.

Figure 3.

Fractured surfaces of the bonded specimens. a, dentin side of fractured specimen bonded with adhesive containing methanol using wet bonding. Most failures occurred between the hybrid layer and the adhesive layer. b, dentin side of fractured specimen bonded with adhesive containing ethanol using solvent-primed bonding. In this group, most of the specimens showed mixed fracture.

Figure 4.

Scanning electron microscopic images of the bonded interfaces after thermocycling. a, the adhesive containing acetone was applied with wet bonding protocol; b, the adhesive containing methanol was applied with wet bonding; c, the adhesive containing methanol was applied on methanol-primed dentin after etching and rinsing procedure. With wet bonding protocol, the interfacial gaps were still observed at the same interface as the specimens observed at 48 hrs. However, with solvent-primed bonding protocol, well-developed hybrid layers and a number of long resin tags were observed without apparent interfacial gap.

Table 1.

Materials used for the preparation of the experimental resin adhesives

Compound Acronym Supplier Batch No.
Bisphenol-A-glycidyl dimethacrylate Bis-GMA Shin-Nakamura chemical Co., Inc. 13431EA
Triethyleneglycol dimethacrylate TEGDMA Shin-Nakamura chemical Co., Inc. 09004BC
Camphoroquinone CQ Aldrich chemical Co., Inc. 00703MN
Ethyl 4-dimethylaminobenzoate 4E Aldrich chemical Co., Inc. 11920PA
*

Other ingredients, such as inhibitor or stabilizer were not included in the experimental resin adhesives.

Table 2.

Microtensile bond strengths of experimental adhesives with different bonding protocols and measuring times (MTBS, unit: MPa)

Adhesives Bonding protocol Measuring time
48 hours 1 month Thermocycling
Ac-containing Solvent primed bonding 14 ± 4.9(13) * 17.4 ± 8.7(17) 18.1 ± 8.3(15)
Wet bonding 9.7 ± 4.3(19) 8.8 ± 3.5(9) 12 ± 5.8(8)
Et-containing Solvent primed bonding 38.9 ± 13(21) 40.4 ± 16.2(17) 50.3 ± 10.2(14)
Wet bonding 33.1 ± 9.2(15) 27.6 ± 12.3(14) 27.6 ± 11.7(14)
Me-containing Solvent primed bonding 15.2 ± 6.8(23) 19.1 ± 8.7(12) 60.7 ± 10.6(10)
Wet bonding 12.8 ± 9.4(19) 22.6 ± 9.7(14) 21.6 ± 4.2(9)

Ac: acetone, Et: ethanol, Me: methanol

*

The numbers in parenthesis are the sample number.