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The effect of solvent evaporation of dentin adhesive on bonding efficacy


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The effect of solvent evaporation of dentin adhesive on bonding efficacy

Article information

Restor Dent Endod. 2010;35(5):321-334
Publication date (electronic) : 2010 September 30
doi : https://doi.org/10.5395/JKACD.2010.35.5.321
Min-Woo Cho, DDS, PhD, Ji-Yeon Kim, DDS, PhD, Duck-Su Kim, DDS, PhD, Kyoung-Kyu Choi, DDS, PhD
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 2010 April 28; Revised 2010 June 19; Accepted 2010 June 29.

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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Copyright © 2010 Korean Academy of Conservative Dentistry

Figure 1

Figure 1

Flowchart of experiment.

Figure 2

Figure 2

Comparison of DE for each adhesive.

Figure 3

Figure 3

Comparison of DC for each adhesive according to DE.

Figure 4

Figure 4

Rea/Ref ratio of One-Step.

Figure 5

Figure 5

Rea/Ref ratio of XP bond.

Figure 6

Figure 6

Rea/Ref ratio of S3 bond.

Figure 7

Figure 7

Rea/Ref ratio of G bond.

Figure 8

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

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

Figure 10

Comparison of µTBS for each experimental group.

Figure 11

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

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

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

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

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

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

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

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

Figure 19

S3 bond over (×5,000).

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

Figure 20

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

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

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 1

Table 2

Experimental groups of 2-step total etching adhesive

Table 2

Table 3

Experimental groups of single-step self etching adhesive

Table 3

Table 4

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

Table 4

Table 5

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

Table 5

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

Table 6

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

Table 6

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