The effect of solvent evaporation of dentin adhesive on bonding efficacy

Min-Woo Cho; Ji-Yeon Kim; Duck-Su Kim; Kyoung-Kyu Choi

doi:10.5395/JKACD.2010.35.5.321

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Basic Research The effect of solvent evaporation of dentin adhesive on bonding efficacy: Min-Woo Cho, DDS, PhD, Ji-Yeon Kim, DDS, PhD, Duck-Su Kim, DDS, PhD, Kyoung-Kyu Choi, DDS, PhD; Journal of Korean Academy of Conservative Dentistry 2010;35(5):321-334.
DOI: https://doi.org/10.5395/JKACD.2010.35.5.321
Published online: September 30, 2010

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; choikkyu@khu.ac.kr

• Received: April 28, 2010 • Revised: June 19, 2010 • Accepted: June 29, 2010

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Abstract
REFERENCES

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

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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).

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, %)

^*The same superscript letters in each adhesive type are statistically not significant.

Table 6

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

^*The same superscript letters in each adhesive type are statistically not significant

Tables & Figures

REFERENCES

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The effect of solvent evaporation of dentin adhesive on bonding efficacy

J Korean Acad Conserv Dent. 2010;35(5):321-334. Published online September 30, 2010

DOI: https://doi.org/10.5395/JKACD.2010.35.5.321

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Figure

The effect of solvent evaporation of dentin adhesive on bonding efficacy

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).

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Figure 22

The effect of solvent evaporation of dentin adhesive on bonding efficacy

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, %)

^*The same superscript letters in each adhesive type are statistically not significant.

Table 6

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

^*The same superscript letters in each adhesive type are statistically not significant

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, %)

^*The same superscript letters in each adhesive type are statistically not significant.

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

^*The same superscript letters in each adhesive type are statistically not significant