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Effect of intermediate resin hydrophilicity on bond strength of single step adhesive
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Original Article Effect of intermediate resin hydrophilicity on bond strength of single step adhesive
Yong-Sung Kim, Sang-Hyuk Park, Gi-Woon Choi, Kyoung-Kyu Choi
Journal of Korean Academy of Conservative Dentistry 2007;32(5):445-458.
DOI: https://doi.org/10.5395/JKACD.2007.32.5.445
Published online: September 30, 2007

Department of Conservative Dentistry, Division of Dentistry, Graduate of Kyung Hee University, Korea.

Corresponding Author: Kyoung-Kyu Choi. Professor of Division of Dentistry, Graduate school of KyungHee University 1, Hoegi Dong, Dongdaemun Gu, Seoul, 130-702, Korea. Tel: 82-2-958-9337, choikkyu@khu.ac.kr
• Received: March 6, 2007   • Revised: April 4, 2007   • Accepted: April 24, 2007

Copyright © 2007 Korean Academy of Conservative Dentistry

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  • The purpose of this study was to evaluate the bond strength of a new Single step system with different curing mode composites, and to evaluate the effect of the intermediate resins which have different hydrophilicity on bonding ability by means of the micro shear bond testing and TEM examination for the adhesive interface. The adhesive used in this study was an experimental single step system (Bisco Inc., Schaumburg, IL). Experimental groups were produced by using six kinds of intermediate resin having different hydrophilicity that was hydrophilic, hydrophobic and most hydrophobic resin and as filled or not after applying adhesive. Each experimental group was further divided into two subgroups whether the adhesive was light cured or not. Dual cured composite (Bis Core, Bisco Ltd., Schaumburg, IL) was placed on the adhesive layer as light cure or self cure mode. The results of bond strength were statistically analyzed using one way ANOVA and multiple comparisons are made using Tukey's test at α < 0.05 level.
    The results of this study were as follows;
    1. The application of intermediate resin did not increase the bond strength for light cured composite.
    2. The bond strength of an experimental adhesive with self cured composite was significantly increased by the application of intermediate resin layer.
    3. The bond strength of adhesive was irrespective of the cure or not of itself before intermediate resin layer applied.
    4. As applied hydrophilic resin layer was, the initial bond strength was higher than both hydrophobic and most hydrophobic one used but there was no significance.
    Using a single step adhesive with dual/self cured composite, the incompatibility between both of them should be solved by the application of intermediate hydrophobic resin to reduce the adhesive permeability. However, Single step adhesive can be used in the light cured composite restoration without any decrease of the initial bond strength.
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Figure 1
Bonding procedure and experimental grouping. LC; light cure, IRL; intermediate resin layer, SC; self cure, HI; hydrophilic, HO; hydrophobic, MO; mostly hydrophobic, f; filled
jkacd-32-445-g001.jpg
Figure 2
A schematic representation of the preparation of serial slabs from bonded composite, the application of nail varnish, immersion in the ammoniacal silver nitrate tracer.
jkacd-32-445-g002.jpg
Figure 3
Bar charts showing the micro shear bond strength for adhesive only (A), with hydrophilic intermediate resin (B), with hydrophobic intermediate resin (C) and with most hydrophobic intermediate resin (D) according to the bonding protocols.
jkacd-32-445-g003.jpg
Figure 4
Bar charts compared to the micro shear bond strengths according to hydrophilicity of intermediate resin.
(A) no filled intermediate resin without cure of adhesive, (B) no filled intermediate resin after cure of adhesive, (C) filled intermediate resin without cure of adhesive, (D) filled intermediate resin after cure of adhesive.
jkacd-32-445-g004.jpg
Figure 5
Transmission electron micrographs of the resin dentin interfaces after immersion in 50wt% silver nitrate. An experimental single step adhesive was bonded with light cure mode composite. A) × 3,400, B) × 7,100: Hybrid layer (H) was formed uniformly between dentin (D) and adhesive layer (A), and its thickness was approximately 2.0 µm. Nanoleakage, in the form of reticular patterns of silver deposits could be seen in the hybrid layer and along dentinal tubule after immersion with silver nitrate tracer.
jkacd-32-445-g005.jpg
Figure 6
TEM micrographs of an experimental adhesive bonded with self cure mode composite. A) The resin dentin interface; The thickness of hybrid layer (H) was not evenly formed. Much of silver deposits were identified within and top of hybrid layer. Adhesive layer (A) was totally separated and silver deposits were infiltrated into adhesive layer (arrows). B) The resin composite interface; The interface was very irregular and worm eaten appearance. The interface of composite (C) side was hollowed with some adhesive and unidentified mass. Some of silver grains were shown along the interface in adhesive side.
jkacd-32-445-g006.jpg
Figure 7
TEM micrographs of the resin dentin interfaces of an experimental adhesive with light cured composite after the hydrophilic intermediate resin layer (IRL) applied. A) IRL was directly applied on adhesive layer without curing. The hybrid layer was well formed and it was hard to identify any silver deposit. The thickness of IRL and adhesive layer was approximately 12 µm. B) IRL was applied after light curing of adhesive layer. Hybrid layer was also well formed and it was hard to identify any silver deposit. The thickness of IRL and adhesive layer was relatively thicker approximately 25 µm. There were definite demarcation line between adhesive layer and IRL (arrows).
jkacd-32-445-g007.jpg
Figure 8
TEM micrographs of the resin dentin interfaces an experimental adhesive with self cured composite after the hydrophilic IRL applied. The IRL was directly applied on adhesive layer without curing. A) × 4,400, B) × 5,600: Hybrid layer was formed evenly and it was also hard to identify any silver deposit. The thickness of hybrid layer was approximately 10 µm.
jkacd-32-445-g008.jpg
Figure 9
TEM micrographs of the resin dentin interfaces an experimental adhesive with light cured composite after the hydrophobic IRL applied (× 8,000). Collagen fibrils within the hybrid layer (H) appeared electron lucent as the undemineralized sections were not stained prior to TEM examination. Nanoleakage, in the form of reticular patterns of silver deposits could be seen in the hybrid layer and along dentinal tubule after immersion with silver nitrate tracer (arrows). Numerous isolated silver grains present throughout the hybrid layer and adhesive layer.
jkacd-32-445-g009.jpg
Figure 10
TEM micrographs of the resin dentin interfaces an experimental adhesive with light cured composite after the most hydrophobic IRL applied (× 12,000). The hybrid layer was well formed and its thickness was approximately 2 µm. Collagen fibrils within the hybrid layer (H) clearly appeared electron lucent at this high magnification. The isolated silver grains were unevenly distributed in both the hybrid layer and lower side of dentinal tubule.
jkacd-32-445-g010.jpg
Figure 11
TEM micrographs of the resin dentin interfaces an experimental adhesive with light cured composite after the most hydrophobic filled IRL applied (×10,000). Nanoleakage, in the form of reticular patterns of silver deposits could be seen in the hybrid layer (arrows). Numerous isolated silver grains were unevenly distributed in both the hybrid layer and dentinal tubule.
jkacd-32-445-g011.jpg
Figure 12
TEM micrographs of the resin dentin interfaces an experimental adhesive with self cured composite after the most hydrophobic filled IRL applied (× 6,000). Nanoleakage, in the form of reticular patterns of silver deposits could be seen in the hybrid layer. Microfiller particles and silver grains could be seen within the intermediate resin layer (I). The adhesive layer (A) was relatively thin (approximately 3 µm) compared to the intermediate resin layer.
jkacd-32-445-g012.jpg
Table 1
The materials used in this study
jkacd-32-445-i001.jpg
Table 2
Micro shear bond strength (MPa, mean ± SD) of an experimental single step adhesive using intermediate resin layer

Same superscript means no statistically difference in each adhesive group at α = 0.05 level. Multiple comparison tests were performed within each adhesive group.

jkacd-32-445-i002.jpg

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      Effect of intermediate resin hydrophilicity on bond strength of single step adhesive
      Image Image Image Image Image Image Image Image Image Image Image Image
      Figure 1 Bonding procedure and experimental grouping. LC; light cure, IRL; intermediate resin layer, SC; self cure, HI; hydrophilic, HO; hydrophobic, MO; mostly hydrophobic, f; filled
      Figure 2 A schematic representation of the preparation of serial slabs from bonded composite, the application of nail varnish, immersion in the ammoniacal silver nitrate tracer.
      Figure 3 Bar charts showing the micro shear bond strength for adhesive only (A), with hydrophilic intermediate resin (B), with hydrophobic intermediate resin (C) and with most hydrophobic intermediate resin (D) according to the bonding protocols.
      Figure 4 Bar charts compared to the micro shear bond strengths according to hydrophilicity of intermediate resin. (A) no filled intermediate resin without cure of adhesive, (B) no filled intermediate resin after cure of adhesive, (C) filled intermediate resin without cure of adhesive, (D) filled intermediate resin after cure of adhesive.
      Figure 5 Transmission electron micrographs of the resin dentin interfaces after immersion in 50wt% silver nitrate. An experimental single step adhesive was bonded with light cure mode composite. A) × 3,400, B) × 7,100: Hybrid layer (H) was formed uniformly between dentin (D) and adhesive layer (A), and its thickness was approximately 2.0 µm. Nanoleakage, in the form of reticular patterns of silver deposits could be seen in the hybrid layer and along dentinal tubule after immersion with silver nitrate tracer.
      Figure 6 TEM micrographs of an experimental adhesive bonded with self cure mode composite. A) The resin dentin interface; The thickness of hybrid layer (H) was not evenly formed. Much of silver deposits were identified within and top of hybrid layer. Adhesive layer (A) was totally separated and silver deposits were infiltrated into adhesive layer (arrows). B) The resin composite interface; The interface was very irregular and worm eaten appearance. The interface of composite (C) side was hollowed with some adhesive and unidentified mass. Some of silver grains were shown along the interface in adhesive side.
      Figure 7 TEM micrographs of the resin dentin interfaces of an experimental adhesive with light cured composite after the hydrophilic intermediate resin layer (IRL) applied. A) IRL was directly applied on adhesive layer without curing. The hybrid layer was well formed and it was hard to identify any silver deposit. The thickness of IRL and adhesive layer was approximately 12 µm. B) IRL was applied after light curing of adhesive layer. Hybrid layer was also well formed and it was hard to identify any silver deposit. The thickness of IRL and adhesive layer was relatively thicker approximately 25 µm. There were definite demarcation line between adhesive layer and IRL (arrows).
      Figure 8 TEM micrographs of the resin dentin interfaces an experimental adhesive with self cured composite after the hydrophilic IRL applied. The IRL was directly applied on adhesive layer without curing. A) × 4,400, B) × 5,600: Hybrid layer was formed evenly and it was also hard to identify any silver deposit. The thickness of hybrid layer was approximately 10 µm.
      Figure 9 TEM micrographs of the resin dentin interfaces an experimental adhesive with light cured composite after the hydrophobic IRL applied (× 8,000). Collagen fibrils within the hybrid layer (H) appeared electron lucent as the undemineralized sections were not stained prior to TEM examination. Nanoleakage, in the form of reticular patterns of silver deposits could be seen in the hybrid layer and along dentinal tubule after immersion with silver nitrate tracer (arrows). Numerous isolated silver grains present throughout the hybrid layer and adhesive layer.
      Figure 10 TEM micrographs of the resin dentin interfaces an experimental adhesive with light cured composite after the most hydrophobic IRL applied (× 12,000). The hybrid layer was well formed and its thickness was approximately 2 µm. Collagen fibrils within the hybrid layer (H) clearly appeared electron lucent at this high magnification. The isolated silver grains were unevenly distributed in both the hybrid layer and lower side of dentinal tubule.
      Figure 11 TEM micrographs of the resin dentin interfaces an experimental adhesive with light cured composite after the most hydrophobic filled IRL applied (×10,000). Nanoleakage, in the form of reticular patterns of silver deposits could be seen in the hybrid layer (arrows). Numerous isolated silver grains were unevenly distributed in both the hybrid layer and dentinal tubule.
      Figure 12 TEM micrographs of the resin dentin interfaces an experimental adhesive with self cured composite after the most hydrophobic filled IRL applied (× 6,000). Nanoleakage, in the form of reticular patterns of silver deposits could be seen in the hybrid layer. Microfiller particles and silver grains could be seen within the intermediate resin layer (I). The adhesive layer (A) was relatively thin (approximately 3 µm) compared to the intermediate resin layer.
      Effect of intermediate resin hydrophilicity on bond strength of single step adhesive

      The materials used in this study

      Micro shear bond strength (MPa, mean ± SD) of an experimental single step adhesive using intermediate resin layer

      Same superscript means no statistically difference in each adhesive group at α = 0.05 level. Multiple comparison tests were performed within each adhesive group.

      Table 1 The materials used in this study

      Table 2 Micro shear bond strength (MPa, mean ± SD) of an experimental single step adhesive using intermediate resin layer

      Same superscript means no statistically difference in each adhesive group at α = 0.05 level. Multiple comparison tests were performed within each adhesive group.


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