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HOME > Restor Dent Endod > Volume 31(6); 2006 > Article
Original Article Aging effect on the microtensile bond strength of self-etching adhesives
JS Park1, JS Kim1,2, MS Kim1, HH Son1,2, HC Kwon1,2, BH Cho1,2
2006;31(6):-426.
DOI: https://doi.org/10.5395/JKACD.2006.31.6.415
Published online: November 30, 2006

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Corresponding author: Byeong-Hoon Cho. Department of Conservative Dentistry, College of Dentistry, Seoul National University, 28 Yeongeon-dong, Chongro-gu Seoul, Korea. 110-749. Tel: 82-2-2072-3514, Fax: 82-2-764-3514, chobh@snu.ac.kr
• Received: April 17, 2006   • Revised: September 12, 2006   • Accepted: September 13, 2006

Copyright © 2006 Korean Academy of Conservative Dentistry

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  • In this study, the changes in the degree of conversion (DC) and the microtensile bond strength (MTBS) of self-etching adhesives to dentin was investigated according to the time after curing. The MTBS of Single Bond (SB, 3M ESPE, USA), Clearfil SE Bond (SE, Kuraray, Japan), Xeno-III (XIII, Dentsply, Germany), and Adper Prompt (AP, 3M ESPE, USA) were measured at 48h, at 1 week and after thermocycling for 5,000 cycles between 5℃ and 55℃. The DC of the adhesives were measured immediately, at 48h and at 7 days after curing using a Fourier Transform Infra-red Spectrometer. The fractured surfaces were also evaluated with scanning electron microscope. The MTBS and DC were significantly increased with time and there was an interaction between the variables of time and material (MTBS, 2-way ANOVA, p = 0.018; DC, Repeated Measures ANOVA, p < 0.001). The low DC was suggested as a cause of the low MTBS of self-etching adhesives, XIII and AP, but the increase in the MTBS of SE and AP after 48h could not be related with the changes in the DC. The microscopic maturation of the adhesive layer might be considered as the cause of increasing bond strength.
  • Keywords: Self-etching adhesive; Microtensile bond strength; Degree of conversion; Brittle fracture; Aging
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Figure 1
Schematic diagram illustrating the procedures for preparing the specimens used in the microtensile bond strength test; bonding and building-up composite crown, grooving and sectioning the bonded sample into hourglass-shaped specimens, and finally testing the specimen fixed on the measuring apparatus.
jkacd-31-415-g001.jpg
Figure 2
Determination of the degree of conversion from mid-IR spectra. The absorbance of aliphatic C=C double bond was measured at 1637 cm-1 (A, before light-curing; B, after light-curing) and the absorbance of (a) aromatic C=C double bond at 1608 cm-1 for Single Bond, SE bond and Adper Prompt, and (b) carbonyl C=O bond at 1720 cm-1 for Xeno III were used as internal references (C, before light-curing; D, after light-curing).
jkacd-31-415-g002.jpg
Figure 3
(a) SEM photograph of the fractured surface of Clearfil SE Bond (dentin side, × 1,000). The fracture surface showed a pattern of brittle fracture, even from the specimens tested at 48h. (b-d) SEM photographs of the fractured surfaces of Adper Prompt (b, dentin side of the specimen fractured at 48h, × 1,000; c, resin side of the specimen fractured at 1 week, × 5,000; d, resin side of the specimen fractured after thermocycling, × 2,000). The fracture surfaces looked brittle with maturation of the adhesive resin layer.
jkacd-31-415-g003.jpg
Figure 4
SEM photographs of the fractured surface of Xeno III. (a) after 48 hours, resin side (× 3,000), (b) after thermocycling, resin side (× 3,000) Lots of porosities were found at the fracture surfaces, which were appeared to be resulted from water inclusion. The surface looked more clearly-fractured after thermocycling than that fractured at 48h.
jkacd-31-415-g004.jpg
Table 1
Dental adhesives used in this study
jkacd-31-415-i001.jpg
Table 2
Compositions of dental adhesives used in this study

Abbreviations:

BHT: 2,6-di-tert-butyl-p-cresol,

CQ: camphorquinone (2,3-bornanedione),

MDP: 10-methacryloxy methacrylate,

HEMA: 2-hydroxylethyl methacrylate,

Pyro-EMA-SK: tetra-methacryl-ethyl-pyrophosphate

PEM-F: Penta-methacryl-oxy-ethyl-cyclo-phosphazen-monofluoride,

UDMA: urethane dimethacrylate,

Bis-GMA: 2,2 bis [4-(2hydroxy3-methacryloyloxy propoxy) phenyl] propane

jkacd-31-415-i002.jpg
Table 3
Microtensile bond strength of dentin adhesives to superficial occlusal dentin at 48 hours and 1 week and after aging with thermocycling (Unit: MPa, mean ± standard deviation, The numbers in parentheses are those of the specimens tested)

*The time at which the microtensile bond strength was measured using a universal testing machine.

**The specimens were thermally cycled 5000 times between 5℃ and 55℃ with 24 seconds of dwell time and 6 seconds of waiting time.

***The same superscript letters mean that there are no significant differences between groups, according to the adhesives (small letters) or the aging method (capital letters).

The results of Two-Way ANOVA suggested that the interaction effect of "adhesive * time" be expected in the measurements of the microtensile bond strength.

jkacd-31-415-i003.jpg
Table 4
The degree of conversion of four adhesives determined by mid-IR spectroscopy (Unit: %, mean ± standard deviation)

*The spectrum of the uncured adhesive was obtained before cure and those of the cured adhesives were obtained immediately after cure and at 48 hours and 1 week after cure.

**The same superscript letters mean that there are no significant differences between groups, according to the adhesives (small letters) or the aging period (capital letters).

§The internal references used for measuring degree of conversion were the absorbance peak at 1608 cm-1 of aromatic -C=C double bond for Single Bond, Clearfil SE Bond and Adper Prompt and that at 1720 cm-1 of carbonyl -C=O double bond for Xeno III, according to their base monomers.

The results of Repeated Measures ANOVA suggested that the interaction effect of "time * adhesive" be expected in the measurements of the degree of conversion.

jkacd-31-415-i004.jpg

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      Aging effect on the microtensile bond strength of self-etching adhesives
      J Korean Acad Conserv Dent. 2006;31(6):415-426.   Published online November 30, 2006
      DOI: https://doi.org/10.5395/JKACD.2006.31.6.415
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    Aging effect on the microtensile bond strength of self-etching adhesives
    Image Image Image Image
    Figure 1 Schematic diagram illustrating the procedures for preparing the specimens used in the microtensile bond strength test; bonding and building-up composite crown, grooving and sectioning the bonded sample into hourglass-shaped specimens, and finally testing the specimen fixed on the measuring apparatus.
    Figure 2 Determination of the degree of conversion from mid-IR spectra. The absorbance of aliphatic C=C double bond was measured at 1637 cm-1 (A, before light-curing; B, after light-curing) and the absorbance of (a) aromatic C=C double bond at 1608 cm-1 for Single Bond, SE bond and Adper Prompt, and (b) carbonyl C=O bond at 1720 cm-1 for Xeno III were used as internal references (C, before light-curing; D, after light-curing).
    Figure 3 (a) SEM photograph of the fractured surface of Clearfil SE Bond (dentin side, × 1,000). The fracture surface showed a pattern of brittle fracture, even from the specimens tested at 48h. (b-d) SEM photographs of the fractured surfaces of Adper Prompt (b, dentin side of the specimen fractured at 48h, × 1,000; c, resin side of the specimen fractured at 1 week, × 5,000; d, resin side of the specimen fractured after thermocycling, × 2,000). The fracture surfaces looked brittle with maturation of the adhesive resin layer.
    Figure 4 SEM photographs of the fractured surface of Xeno III. (a) after 48 hours, resin side (× 3,000), (b) after thermocycling, resin side (× 3,000) Lots of porosities were found at the fracture surfaces, which were appeared to be resulted from water inclusion. The surface looked more clearly-fractured after thermocycling than that fractured at 48h.

    Figure 1

    Figure 2

    Figure 3

    Figure 4

    Aging effect on the microtensile bond strength of self-etching adhesives

    Dental adhesives used in this study

    Compositions of dental adhesives used in this study

    Abbreviations:

    BHT: 2,6-di-tert-butyl-p-cresol,

    CQ: camphorquinone (2,3-bornanedione),

    MDP: 10-methacryloxy methacrylate,

    HEMA: 2-hydroxylethyl methacrylate,

    Pyro-EMA-SK: tetra-methacryl-ethyl-pyrophosphate

    PEM-F: Penta-methacryl-oxy-ethyl-cyclo-phosphazen-monofluoride,

    UDMA: urethane dimethacrylate,

    Bis-GMA: 2,2 bis [4-(2hydroxy3-methacryloyloxy propoxy) phenyl] propane

    Microtensile bond strength of dentin adhesives to superficial occlusal dentin at 48 hours and 1 week and after aging with thermocycling (Unit: MPa, mean ± standard deviation, The numbers in parentheses are those of the specimens tested)

    *The time at which the microtensile bond strength was measured using a universal testing machine.

    **The specimens were thermally cycled 5000 times between 5℃ and 55℃ with 24 seconds of dwell time and 6 seconds of waiting time.

    ***The same superscript letters mean that there are no significant differences between groups, according to the adhesives (small letters) or the aging method (capital letters).

    The results of Two-Way ANOVA suggested that the interaction effect of "adhesive * time" be expected in the measurements of the microtensile bond strength.

    The degree of conversion of four adhesives determined by mid-IR spectroscopy (Unit: %, mean ± standard deviation)

    *The spectrum of the uncured adhesive was obtained before cure and those of the cured adhesives were obtained immediately after cure and at 48 hours and 1 week after cure.

    **The same superscript letters mean that there are no significant differences between groups, according to the adhesives (small letters) or the aging period (capital letters).

    §The internal references used for measuring degree of conversion were the absorbance peak at 1608 cm-1 of aromatic -C=C double bond for Single Bond, Clearfil SE Bond and Adper Prompt and that at 1720 cm-1 of carbonyl -C=O double bond for Xeno III, according to their base monomers.

    The results of Repeated Measures ANOVA suggested that the interaction effect of "time * adhesive" be expected in the measurements of the degree of conversion.
    Table 1 Dental adhesives used in this study

    Table 2 Compositions of dental adhesives used in this study

    Abbreviations:

    BHT: 2,6-di-tert-butyl-p-cresol,

    CQ: camphorquinone (2,3-bornanedione),

    MDP: 10-methacryloxy methacrylate,

    HEMA: 2-hydroxylethyl methacrylate,

    Pyro-EMA-SK: tetra-methacryl-ethyl-pyrophosphate

    PEM-F: Penta-methacryl-oxy-ethyl-cyclo-phosphazen-monofluoride,

    UDMA: urethane dimethacrylate,

    Bis-GMA: 2,2 bis [4-(2hydroxy3-methacryloyloxy propoxy) phenyl] propane

    Table 3 Microtensile bond strength of dentin adhesives to superficial occlusal dentin at 48 hours and 1 week and after aging with thermocycling (Unit: MPa, mean ± standard deviation, The numbers in parentheses are those of the specimens tested)

    *The time at which the microtensile bond strength was measured using a universal testing machine.

    **The specimens were thermally cycled 5000 times between 5℃ and 55℃ with 24 seconds of dwell time and 6 seconds of waiting time.

    ***The same superscript letters mean that there are no significant differences between groups, according to the adhesives (small letters) or the aging method (capital letters).

    The results of Two-Way ANOVA suggested that the interaction effect of "adhesive * time" be expected in the measurements of the microtensile bond strength.

    Table 4 The degree of conversion of four adhesives determined by mid-IR spectroscopy (Unit: %, mean ± standard deviation)

    *The spectrum of the uncured adhesive was obtained before cure and those of the cured adhesives were obtained immediately after cure and at 48 hours and 1 week after cure.

    **The same superscript letters mean that there are no significant differences between groups, according to the adhesives (small letters) or the aging period (capital letters).

    §The internal references used for measuring degree of conversion were the absorbance peak at 1608 cm-1 of aromatic -C=C double bond for Single Bond, Clearfil SE Bond and Adper Prompt and that at 1720 cm-1 of carbonyl -C=O double bond for Xeno III, according to their base monomers.

    The results of Repeated Measures ANOVA suggested that the interaction effect of "time * adhesive" be expected in the measurements of the degree of conversion.

    Table 1

    Table 2

    Table 3

    Table 4

    Restor Dent Endod : Restorative Dentistry & Endodontics
    © The Korean Academy of Conservative Dentistry.
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