Open Access, Peer-reviewed
eISSN 2234-7666
    J Korean Acad Conserv Dent. 2010 Sep;35(5):321-334. Korean.
    Published online Sep 30, 2010.
    https://doi.org/10.5395/JKACD.2010.35.5.321
    Copyright © 2010 Korean Academy of Conservative Dentistry
    Original Article

    The effect of solvent evaporation of dentin adhesive on bonding efficacy

    Min-Woo Cho, DDS, PhD, Student , Ji-Yeon Kim, DDS, PhD, Student , Duck-Su Kim, DDS, PhD, Clinical Instructor and Kyoung-Kyu Choi, DDS, PhD, Professor
      • Division of Dentistry, Department of Conservative Dentistry, Graduate of Kyung Hee University, Seoul, Korea.
    • Correspondence to Kyoung-Kyu Choi, DDS, PhD. Professor, Division of Dentistry, Graduate school of Kyung Hee University, 1, Hoegi-dong, Dongdaemun-gu, Seoul, Korea 130-702. Tel, +82-2-958-9337; Fax, +82-2-960-5108; Email: choikkyu@khu.ac.kr
    Received April 28, 2010; Revised June 19, 2010; Accepted June 29, 2010.

    Abstract

    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 µTBS 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 S3 bond. In µTBS 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.

    Keywords
    Bonding efficacy; Degree of conversion; Degree of evaporation; Dentin adhesive; Raman spectroscopy; Residual solvent

    Figures

    Figure 1
    Flowchart of experiment.

    Figure 2
    Comparison of DE for each adhesive.

    Figure 3
    Comparison of DC for each adhesive according to DE.

    Figure 4
    Rea/Ref ratio of One-Step.

    Figure 5
    Rea/Ref ratio of XP bond.

    Figure 6
    Rea/Ref ratio of S3 bond.

    Figure 7
    Rea/Ref ratio of G bond.

    Figure 8
    µTBS of experimental group (2-step total etching adhesive).

    *The same letters within graph are statistically not significant, *Error bar means SD.

    Figure 9
    µTBS of experimental group (single-step self etching adhesive).

    *The same letters within graph are statistically not significant, *Error bar means SD.

    Figure 10
    Comparison of µTBS for each experimental group.

    Figure 11
    One-Step under (×5,000).

    Incomplete hybrid layer was observed (between vertical arrow). Resin tags were poorly formed (R, composite resin; D, dentin).

    Figure 12
    One-Step control (×5,000).

    Complete hybrid layer and uniform resin tags could be noticed (R, composite resin; D, dentin; HL, hybrid layer).

    Figure 13
    One-Step over (×5,000).

    Resin tags were well formed but adhesive resin was not certain. Notice continuous gap between composite resin and dentin (oblique arrows)(R, composite resin; D, dentin).

    Figure 14
    XP bond under (×5,000).

    Resin tags were well formed. The thickness of adhesive resin was 2-3 µm and clearly distinct (between vertical arrow)(R, composite resin; D, dentin; A, adhesive resin).

    Figure 15
    XP bond control (×5,000).

    Complete hybrid layer and uniform resin tags could be noticed (R, composite resin; D, dentin; HL, hybrid layer).

    Figure 16
    XP bond over (×5,000).

    Complete hybrid layer and uniform resin tags could be noticed. adhesive resin was thinner than under group (R, composite resin; D, dentin; HL, hybrid layer).

    Figure 17
    S3 bond under (×5,000).

    Hybrid layer was not certain but tight connection could be noticed. The small number of slender resin tags were observed (R, composite resin; D, dentin).

    Figure 18
    S3 bond control (×5,000).

    The number of resin tags were slightly higher than under group but there was no clear difference between control and under group (R, composite resin; D, dentin).

    Figure 19
    S3 bond over (×5,000).

    There was no clear difference between control and over group (R, composite resin; D, dentin).

    Figure 20
    G bond under (×5,000).

    Large and continuous gap was formed (vertical arrows), droplets were formed in adhesive resin (oblique arrows) (R, composite resin; D, dentin; A, adhesive resin).

    Figure 21
    G bond control (×5,000).

    Hybrid layer was not certain but tight connection could be noticed. The small number of resin tags were observed (R, composite resin; D, dentin).

    Figure 22
    G bond over (×5,000).

    There was no clear difference between control and over group (R, composite resin; D, dentin).

    Tables

    Table 1
    Adhesives used in this study

    Table 2
    Experimental groups of 2-step total etching adhesive

    Table 3
    Experimental groups of single-step self etching adhesive

    Table 4
    Degree of evaporation (DE) of each adhesive (Mean ± SD, %)

    Table 5
    Degree of conversion (DC) of each adhesive (Mean ± SD, %)

    Table 6
    µTBS for each experimental group (Mean ± SD, MPa)

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    MeSH Terms
    Acetone
    Adhesives
    Dentin
    Ethanol
    Oxygen
    Solvents
    Spectrum Analysis
    Spectrum Analysis, Raman
    Weight Loss
    Metrics
    Share
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