JAD Smear Layer
JAD Smear Layer
JAD Smear Layer
RESEARCH
Purpose: To evaluate the effects of different smear layers on the microtensile bond strength (μTBS) of a reference
two-step self-etch adhesive and two universal adhesives.
Materials and Methods: Mid-coronal dentin of 90 teeth was exposed and divided into three bur groups (coarse dia-
mond, fine diamond, or tungsten carbide). Each bur-prepared group was further divided into three adhesive groups:
Clearfil SE Bond (SE, Kuraray Noritake), Single Bond Universal (SB; 3M Oral Care), and G-Premio Bond (GP, GC).
After adhesive application, 4-mm-thick resin composites were built up. Half of the teeth in each bur-adhesive group
were used in immediate μTBS testing, and the others were tested after thermal aging (n = 5). Rectangular sticks
were prepared using a low-speed diamond saw. For each tooth, 6 central sticks were used in the μTBS test. Statis-
tical analysis was performed using three-way ANOVA and Bonferroni tests (α = 0.05).
Results: SE presented higher μTBS than universal adhesives and SB presented higher μTBS than GP regardless of
dentin surface preparation and thermal aging (p ˂ 0.05). For SE and SB, the tungsten carbide bur demonstrated
higher immediate and aged μTBS than did the extra-fine diamond bur (p ˂ 0.05). The immediate μTBS was similar
for GP with all bur types (p ˃ 0.05); the tungsten carbide and extra-fine diamond burs presented higher μTBS than
did the coarse-diamond bur after thermal aging (p ˂ 0.05).
Conclusion: Dentin surface preparation and adhesive type had significant effects on μTBS. The smear layer created
with an extra-fine diamond or tungsten carbide bur is favorable when mild and ultra-mild self-etch adhesives are used.
Keywords: smear layer, universal adhesive, self-etch adhesives, bond strength, microtensile bond strength.
J Adhes Dent 2022; 24: 87–94. Submitted for publication: 01.01.21; accepted for publication: 17.01.22
doi: 10.3290/j.jad.b2838121
doi: 10.3290/j.jad.b2838121 87
Hatırlı et al
Clearfil SE Bond Two-step mild Primer: 10-MDP, HEMA, hydrophilic 2.0 Apply primer for 20 s.
(Kuraray Noritake; Tokyo, self-etch dimethacrylate, di-camphorquinone, (primer) Dry with mild air flow.
Japan) N,N-diethanol-p-toluine, water Apply bonding.
Bond: 10-MDP, bis-GMA, HEMA, hydrophobic Gently air dry.
dimethacrylate, di-camphorquinone, Light cure for 10 s.
N,N-diethanol-p-toluine, silanated colloidal
silica
G-Premio Bond Semi-strong 10-MDP, 4-META, 10-methacryoyloxydecyl 1.5 Apply using a microbrush.
(GC; Tokyo, Japan) self-etch dihydrogen thiophosphate, methacrylate Leave undisturbed for 10 s after
adic ester, distilled water, acetone, photo- application.
initiators, silica fine powder Dry thoroughly for 5 s with oil-free air
under maximum air pressure.
Light cure for 10 s.
Single Bond Universal Ultra-mild 10-MDP, HEMA, silane, dimethacrylate 2.7 Apply the adhesive to the entire
(3M Oral Care; St Paul, self-etch resins, VitrebondTM copolymer, filler, surface and rub it in for 20 s.
MN, USA) ethanol, water, initiators Gently air dry the adhesive for
approximately 5 s for the solvent to
evaporate.
Light cure for 10 s.
10-MDP: 10-methacryloxydecyl dihydrogen phosphate; HEMA: 2-hydroxyethyl methacrylate; bis-GMA: bisphenol A diglycidyl methacrylate; 4-META: 4-methacryloyloxyethyl
trimellitate anhydrate.
SL can be considered an obstacle to the infiltration of 20-KAEK-209). Ninety-three extracted human third molars that
self-etch adhesives and should be adequately dealt with.15 were free of caries, cracks, or fractures were used in this study.
The importance of the cavity preparation method has been All teeth were stored in an aqueous solution of 0.5% chlora-
highlighted in previous studies, owing to the fact that thicker mine-T at 4°C and were used within 6 months of extraction.
SL impairs the effectiveness of mild and ultra-mild self-etch Ninety teeth that were used for the μTBS test were em-
adhesives.22,28 Various in vitro studies have observed the bedded in a self-curing acrylic resin (Imicryl; Konya, Turkey).
effects of the types of SL on the bonding efficacy of self- Occlusal surfaces of the teeth were cut using a low-speed
etch adhesives to enamel and dentin.4,6,8,11,20,22,23 How- diamond saw (Microcut 125, Metkon; Bursa, Turkey) under
ever, there is no consensus on the effect of SL type on the continuous cooling with a water and cutting-fluid mixture
adhesive performance of self-etch adhesives. Two-step self- (Metcool II, Metkon) to expose the mid-coronal dentin. The
etch and strong or semi-strong 1-step self-etch adhesives dentin surfaces were examined for the presence of enamel
do not appear to be substantially influenced by the type of or exposure of the pulp. The teeth were randomly divided
SL.8,24 In contrast, for mild or ultra-mild 1-step self-etch ad- into three groups (n = 30) according to the following dentin
hesives, the effect of SL type depends on the formulation surface preparation procedures:
and pH of the adhesive. Previous studies have reported that y Group 1: A cylindrical coarse-grit diamond bur (107–
thicker SLs have a negative effect of on the bond 181 μm, 852 FG Meisinger, Hager & Meisinger; Neuss,
strength.8,22 In addition, the available knowledge on univer- r Germany) at high speed with copious water cooling.
sal adhesives with respect to this aspect is limited. y Group 2: First, the dentin surfaces were prepared as in
Therefore, this study aimed to evaluate the effects of group 1, followed by a cylindrical extra-fine grit diamond
clinically relevant SLs on the microtensile bond strength bur (10–36 μm, 852 FG Meisinger) at high speed with
(μTBS) of a reference 2-step self-etch adhesive and two dif- f copious water cooling.
ferent universal adhesives applied in self-etch mode. The y Group 3: A cylindrical 8-fluted tungsten carbide bur
null hypotheses tested were: 1) there is no effect of the (HM21R Meisinger) at low speed with the handpiece run-
type of adhesive, 2) no effect of different SLs created with ning at 10,000 rpm with copious water cooling.
different burs, and 3) there is no negative effect of thermal
aging on the μTBS of the tested adhesives. Five strokes were applied with light pressure using the
burs to create uniform dentin surfaces.21
After surface preparation, adhesive procedures were per- r fixed onto a modified Geraldeli’s jig in a μTBS testing appa-
formed immediately. The material compositions and appli- ratus using cyanoacrylate glue. Subsequently, the speci-
cation steps suggested by the manufacturers are listed in mens were subjected to tensile force in a universal testing
Table 1. After adhesive application and polymerization, machine (Shimadzu; Kyoto, Japan) at a cross-head speed of
4-mm-thick resin composites (Filtek Z250; 3M Oral Care) 1 mm/min. The μTBS was calculated in MPa by dividing the
were built up on the bonded dentin surfaces in 2-mm incre- fracture force by the bonded area. The Academy of Dental
ments. Each layer was light cured using an LED light-curing Materials guidelines on the μTBS test protocol were strictly
unit (20 s, 1000 mW/cm2, Valo, Ultradent; South Jordan, followed during specimen preparation and testing.2
UT, USA). Dentin preparation, adhesive application, and
resin composite build-up procedures were all performed by Failure Mode Analysis
the same operator to ensure standardization. All the fractured specimen surfaces were examined stereomi-
After the application of resin composite buildups, the croscopically (Stemi C-2000, Zeiss; Oberkochen, Germany) to
specimens were kept in distilled water at 37°C for 24 h. determine the mode of failure (adhesive interfacial failure,
Half of the teeth in each bur-adhesive group (n = 5) under-
r cohesive failure in resin composite, cohesive failure in den-
went immediate μTBS testing. Before testing, the remaining tin, or mixed failure). Two representative samples of each
half were thermally aged in a thermocycler (SD Mechatronik experimental group with a μTBS close to the mean were
Thermocycler, SD Mechatronik; Westerham, Germany) for selected and subsequently imaged using field emission
25,000 cycles with 20 s of immersion at each temperature scanning electron microscopy (FE-SEM, Mira 3 XMU, Tescan;
(5°C and 55°C) and a 5-s transfer time between baths. Brno, Czech Republic).
doi: 10.3290/j.jad.b2838121 89
Hatırlı et al
g h i
G Premio Bond
h j l
(p ˂ 0.05), of which SB had higher μTBS than did GP, irrespec- with the coarse diamond displayed a rough surface and ir- r
tive of dentin surface preparation and thermal aging regular grooves. The grooves were shorter and narrower when
(p ˂ 0.05). For each adhesive, the immediate μTBSs of the the extra-fine diamond bur was used. The dentin surface pre-
groups were similar to that of post-aging μTBS, except for pared with the tungsten-carbide bur exhibited wide, uniform
GP applied on extra-fine bur- and tungsten-carbide-prepared grooves. FE-SEM images revealed that SL covered the dentin
dentin surfaces, which presented higher μTBS values after surfaces and smear plugs occluded the orifices of dentin tu-
thermal aging (p ˂ 0.05). bules. Representative FE-SEM images of adhesive-dentin
For SE and SB, tungsten carbide bur groups exhibited interfacial structures of each group are shown in Fig 3. For
both higher immediate and aged μTBS values than did the SE, long resin tags inside the dentin tubules were observed
extra-fine grit diamond bur (p ˂ 0.05). The difference be- using FE-SEM. However, for SB and GP, the resin tags were
tween the coarse and extra-fine burs was not significant few and short. In addition, GP presented 1- to 5-μm round
(p ˃ 0.05). In addition, the immediate μTBSs were similar gaps, whereas SB presented smaller gaps of up to 1 μm.
for GP irrespective of the burs used (p ˃ 0.05). However, for For GP, in some of the resin composite-adhesive interfaces,
GP, the 8-fluted tungsten carbide bur and extra-fine diamond line-shaped separations were observed (Figs 1 and 3).
bur groups presented higher μTBSs than did the coarse-grit
diamond bur group after thermal aging (p ˂ 0.05).
DISCUSSION
Fracture Mode Analysis
The number of fracture modes for each group is listed in This study assessed the effects of clinically relevant SLs,
Table 3. The most frequent fracture modes were adhesive created using different burs, on the immediate and ther-
(333/540) and mixed (131/540). A clear tendency for co- mally aged μTBS of a reference 2-step self-etch, a semi-
hesive failures was observed in the groups that presented strong, and an ultra-mild universal adhesive. The results of
higher μTBSs. Cohesive failures mostly occurred in the SE this study revealed that dentin surface preparation and ad-
(40/120) and SB (28/120) groups. The main failure mode hesive type had significant effects on μTBS. Therefore, the
was adhesive for GP (93/120). When adhesive failures null hypothesis that there is no effect of 1) type of adhesive
were examined by FE-SEM at 2500X magnification, numer- and 2) SLs created with different burs was rejected.
ous pores on the entire surface were observed for GP The SL can be considered a physical barrier that consid-
(Fig 1). erably influences bonding performance,4,8 owing to the divi-
sion of the hybrid layer into an upper, resin-infiltrated demin-
FE-SEM of Prepared Dentin Surface and Interfacial eralized smear layer, and a lower, true hybrid layer.12 In
Structure addition, SL characteristics are directly affected by the type
Representative FE-SEM images of bur-prepared dentin sur-r of rotary instrument, cutting speed, and grit size of the burs
faces are presented in Fig 2. The dentin surface prepared used (Fig 2).12 To create a clinically relevant SL for bond
doi: 10.3290/j.jad.b2838121 91
Hatırlı et al
m o r
G Premio Bond
n p s
strength tests, 8-fluted carbide and medium-grit diamond monomers might not penetrate uniformly. However, the im-
burs for direct bonding and fine-grit diamond burs for indi- mediate μTBS of the semi-strong universal adhesive (GP)
rect bonding are recommended.2 When using diamond burs was not affected by the type of SL. This might be explained
at high speeds, a SL with higher density is created than by the strong acidity of the adhesive.
with SiC papers,16,22 and the SL thickness increases with The pH values of self-etch adhesives can significantly
the increasing coarseness of the diamond bur.21 Dias et al6 influence the dissolution of the SL and etching of the den-
observed that diamond burs at high speed produce a tin surface.24 Universal adhesives differ from each other in
rougher surface and that the use of carbide burs can en- acidity; the bond strength to dentin along with the bond
hance bond strength. However, the effects of diamond and stability have been shown to depend on acidity.5 Therefore,
carbide burs on the bond strength and durability of univer- r this study tested universal adhesives with quite different
sal adhesives have not been elucidated. pH values: a semi-strong (GP; pH: 1.5) and an ultra-mild
One of the major concerns with self-etch adhesives is (SB; pH: 2.7) adhesive, as well as the reference mild two-
the potential interference of the SL created by the bur dur-r step self-etch adhesive (SE), according to the classification
ing cavity preparation. The results of present study revealed by Van Meerbeek et al.15 The higher pH of the ultra-mild
that the reference mild 2-step self-etch adhesive (SE) and universal adhesive (SB) would be expected to result in re-
the ultra-mild universal adhesive (SB) yielded significantly duced etching ability, be less able to etch different SL
higher μTBS on SL created with a tungsten carbide bur than types, and reduce demineralization of the dentin surface,
on SL created with a coarse-grit diamond bur (p ˂ .05). which is beneficial for micromechanical interlocking. How-
Saikaew et al20 stated that the acidic monomers of self- ever, consistent with the findings of previous studies, SB
etch adhesives are buffered and their acidity is decreased showed a higher μTBS than the other universal adhesive,
by the SL. They also confirmed that in the thicker and more GP, for all SL types.24 This might be explained by the differ-
compact SL created with regular-grit diamond bur, acidic ences in ingredients, such as solvent and functional mono-
doi: 10.3290/j.jad.b2838121 93
Hatırlı et al
16. Oliveira SS, Pugach MK, Hilton JF, Watanabe LG, Marshall SJ, Marshall Jr 28. Van Meerbeek B, Yoshihara K, Yoshida Y, Mine A, De Munck J, Van Landuyt
GW. The influence of the dentin smear layer on adhesion: a self-etching K. State of the art of self-etch adhesives. Dent Mater 2011;27:17–28.
primer vs. a total-etch system. Dent Mater 2003;19:758–767. 29. Wagner A, Wendler M, Petschelt A, Belli R, Lohbauer U. Bonding perfor- r
17. Oz FD, Kutuk ZB, Balkan E, Ozturk C, Gurgan S. Bond strength of three mance of universal adhesives in different etching modes. J Dent 2014;
different universal adhesives after different thermal cycling protocols. J 42:800–807.
Adhes Sci Technol 2018;32:2741–2752. 30. Yamada M, Miyazaki M, Moore BK. Influence of interchanging adhesive
18. Perdigao J, Lambrechts P, Van Meerbeek B, Vanherle G, Lopes A. Field resins and self-etching primers on the mechanical properties of adhesive
emission SEM comparison of four postfixation drying techniques for resins. Oper Dent 2004;29:532–537.
human dentin. J Biomed Mater Res 1995;29:1111–1120. 31. Yiu CK, Pashley EL, Hiraishi N, King NM, Goracci C, Ferrari M, Carvalho
19. Sai K, Shimamura Y, Takamizawa T, Tsujimoto A, Imai A, Endo H, Bark- RM, Pashley DH, Tay FR. Solvent and water retention in dental adhesive
meier WW, Latta MA, Miyazaki M. Influence of degradation conditions on blends after evaporation. Biomaterials 2005;26:6863–6872.
dentin bonding durability of three universal adhesives. J Dent 2016;54: 32. Yoshida Y, Yoshihara K, Nagaoka N, Hayakawa S, Torii Y, Ogawa T, Osaka
56–61. A, Van Meerbeek B. Self-assembled nano-layering at the adhesive inter- r
20. Saikaew P, Chowdhury AA, Fukuyama M, Kakuda S, Carvalho RM, Sano H. face. J Dent Res 2012;91:376–381.
The effect of dentine surface preparation and reduced application time of 33. Yoshihara K, Nagaoka N, Nakamura A, Hara T, Yoshida Y, Van Meerbeek B.
adhesive on bonding strength. J Dent 2016;47:63–70. Nano-layering adds strength to the adhesive interface. J Dent Res 2021;
21. Saikaew P, Matsumoto M, Chowdhury A, Carvalho R, Sano H. Does short- 100:515–521.
ened application time affect long-term bond strength of universal adhe- 34. Yoshihara K, Yoshida Y, Hayakawa S, Nagaoka N, Irie M, Ogawa T, Van
sives to dentin? Oper Dent 2018;43:549–558. Landuyt KL, Osaka A, Suzuki K, Minagi S, Van Meerbeek B. Nanolayering
22. Saikaew P, Senawongse P, AFM A, Sano H, Harnirattisai C. Effect of smear of phosphoric acid ester monomer on enamel and dentin. Acta Biomater
layer and surface roughness on resin-dentin bond strength of self-etching 2011;7:3187–3195.
adhesives. Dent Mater J 2018;37:973–980.
23. Sattabanasuk V, Vachiramon V, Qian F, Armstrong SR. Resin–dentin bond
strength as related to different surface preparation methods. J Dent
2007; 35:467–475.
24. Takamizawa T, Barkmeier WW, Sai K, Tsujimoto A, Imai A, Erickson RL,
Latta MA, Miyazaki M. Influence of different smear layers on bond durabil-
ity of self-etch adhesives. Dent Mater 2018;34:246–259.
25. Tao L PD, Boyd L. Effect of different types of smear layers on dentin and Clinical relevance: Smear layer type, pH, and formula-
enamel shear bond strengths. Dent Mater 1988;4:208–216.
tion of the adhesive can influence the dentin bond
26. Ting S, Chowdhury AA, Pan F, Fu J, Sun J, Kakuda S, Hoshika S, Matsuda
Y, Ikeda T, Nakaoki Y, Abe S, Yoshida Y, Sano H. Effect of remaining dentin strength of self-etch adhesives. Finishing preparation
thickness on microtensile bond strength of current adhesive systems. with tungsten carbide burs instead of coarse diamond
Dent Mater J 2015;34:181–188.
burs for direct bonding, and extra-fine diamond burs for
27. Van Landuyt K, Snauwaert J, De Munck J, Coutinho E, Poitevin A, Yoshida
Y, Suzuki K, Lambrechts P, Van Meerbeek B. Origin of interfacial droplets indirect bonding, can be recommended.
with one-step adhesives. J Dent Res 2007;86:739–744.