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Journal <strong>of</strong> Dentistry (2006) 34, 283–291<br />

<strong>Microtensile</strong> <strong>bond</strong> <strong>strength</strong> <strong>of</strong> a <strong>filled</strong> <strong>vs</strong> un<strong>filled</strong><br />

<strong>adhesive</strong> <strong>to</strong> <strong>dentin</strong> using self-etch and<br />

<strong>to</strong>tal-etch technique<br />

Esra Can Say a, *, Masa<strong>to</strong>shi Nakajima b , Pisol Senawongse c ,Mübin Soyman a ,<br />

Füsun Özer d , Miwako Ogata b , Junji Tagami b,e<br />

a<br />

Department <strong>of</strong> Operative Dentistry, Faculty <strong>of</strong> Dentistry, Yeditepe University, Istanbul, Turkey<br />

b<br />

Department <strong>of</strong> Res<strong>to</strong>rative Sciences, Cariology and Operative Dentistry, Graduate School, Tokyo Medical<br />

and Dental University, Tokyo, Japan<br />

c<br />

Department <strong>of</strong> Operative Dentistry, Mahidol University, Bangkok, Thailand<br />

d<br />

Department <strong>of</strong> Operative Dentistry, Faculty <strong>of</strong> Dentistry, Selcuk University, Konya, Turkey<br />

e<br />

Center <strong>of</strong> Excellence Program for Frontier Research on Molecular Destruction and Reconstruction <strong>of</strong> Tooth<br />

and Bone, Tokyo Medical and Dental University, Tokyo, Japan<br />

Received 9 April 2005; received in revised form 8 July 2005; accepted 14 July 2005<br />

KEYWORDS<br />

Filled <strong>adhesive</strong>;<br />

Un<strong>filled</strong> <strong>adhesive</strong>;<br />

Total-etch;<br />

Self-etch<br />

* Corresponding author. Tel.: C90 2163636044; fax: C90<br />

2163636211.<br />

E-mail address: esracansay@yahoo.com (E. Can Say).<br />

0300-5712/$ - see front matter Q 2005 Elsevier Ltd. All rights reserved.<br />

doi:10.1016/j.jdent.2005.07.003<br />

www.intl.elsevierhealth.com/journals/jden<br />

Summary Objective: The purpose <strong>of</strong> this study was <strong>to</strong> evaluate the effect <strong>of</strong> a <strong>filled</strong><br />

<strong>adhesive</strong> (One-Step Plus; Bisco) versus an un<strong>filled</strong> <strong>adhesive</strong> (One-Step; Bisco) on the<br />

microtensile <strong>bond</strong> <strong>strength</strong> (mTBS) <strong>to</strong> <strong>dentin</strong> using <strong>to</strong>tal-etch (Uni-etch; Bisco) and<br />

self-etch (Tyrian SPE; Bisco) techniques.<br />

Methods: Twenty extracted human third molars were ground flat <strong>to</strong> expose occlusal<br />

<strong>dentin</strong>. After the <strong>dentin</strong> surfaces were polished with 600-grit SiC paper, the teeth<br />

were randomly assigned <strong>to</strong> four groups according <strong>to</strong> the <strong>bond</strong>ing agent and technique<br />

being used. Dentin surfaces were <strong>bond</strong>ed with One-Step PlusC<strong>to</strong>tal-etch; One-Step<br />

PlusCself-etch; One-StepC<strong>to</strong>tal-etch and One-StepCself-etch. Composite buildups<br />

were performed with Clearfil AP-X (Kuraray Medical). Following s<strong>to</strong>rage in distilled<br />

water at 37 8C for 24 h, the <strong>bond</strong>ed specimens were serially sectioned in<strong>to</strong> 0.7 mmthick<br />

slabs and then trimmed <strong>to</strong> hour-glass shapes with a 1 mm 2 cross-sectional area<br />

(nZ20). <strong>Microtensile</strong> <strong>bond</strong> <strong>strength</strong>s were determined using the EZ-test (Shimadzu)<br />

at a cross-head speed <strong>of</strong> 1 mm/min. Data were analyzed using two-way ANOVA and<br />

Tukey’s post hoc test.<br />

Results: There were no significant differences in the mTBS between One-Step Plus<br />

and One-Step <strong>adhesive</strong>s when they were used with the <strong>to</strong>tal-etch and self-etch<br />

techniques (pO0.05). However with the <strong>to</strong>tal-etch technique both <strong>adhesive</strong>s yielded<br />

significantly higher <strong>bond</strong> <strong>strength</strong> values than the self-etch technique (p!0.001).


284<br />

Introduction<br />

Resin composites with <strong>adhesive</strong> materials have<br />

been available on the dental market for about<br />

four decades and are widely used for both anterior<br />

and posterior res<strong>to</strong>rations due <strong>to</strong> the esthetic<br />

demands <strong>of</strong> patients, however they still have<br />

some undesirable properties. One is the polymerization<br />

shrinkage which produces contraction stresses<br />

generally concentrate at the <strong>bond</strong>ing<br />

interface. 1 If these stresses exceed the <strong>bond</strong><br />

<strong>strength</strong> <strong>to</strong> <strong>dentin</strong>, an interfacial gap will be<br />

formed, leading <strong>to</strong> bacterial infiltration, sensitivity,<br />

secondary caries and possible pulpal damage. 2<br />

Thicker <strong>adhesive</strong> layers or liners may act as an<br />

elastic intermediate layer (elastic cavity wall)<br />

between the cavity walls and the adjacent composite.<br />

That is, they could resist the polymerization<br />

shrinkage stress <strong>of</strong> the resin composites 1 and absorb<br />

the shock produced by occlusal loads and thermal<br />

cycling. 3 Using un<strong>filled</strong> <strong>adhesive</strong>s, thicker layers are<br />

not recommended because these materials have<br />

lower mechanical properties and usually provide no<br />

radioopacity which could mislead clinicians <strong>to</strong><br />

interprete the <strong>adhesive</strong> radiotransparency as gap<br />

formation or recurrent caries at the margin <strong>of</strong> the<br />

res<strong>to</strong>ration. 4 Based on this idea, <strong>filled</strong> <strong>adhesive</strong>s<br />

have been introduced, 5–7 which have included<br />

various types <strong>of</strong> fillers; such as conventional glass,<br />

ion leachable glass, silica and nanometer-sized<br />

aerosil silica fillers. 8–10 They have been reported<br />

<strong>to</strong> improve marginal and internal seal <strong>of</strong> composite<br />

res<strong>to</strong>rations 6,11–13 and have sufficient radioopacity<br />

<strong>to</strong> be discernible on dental X-ray films. 7<br />

Current <strong>adhesive</strong> systems employ two simplified<br />

application procedures <strong>to</strong> achieve the goal <strong>of</strong><br />

micromechanical retention between resin and<br />

<strong>dentin</strong>. The first method attempts <strong>to</strong> remove the<br />

smear layer completely via acid etching and rinsing,<br />

followed by the application <strong>of</strong> an <strong>adhesive</strong> agent on<br />

a wet <strong>dentin</strong> surface; the <strong>to</strong>tal-etch technique. 14<br />

The second category is the self-etch technique,<br />

which simultaneously demineralizes <strong>dentin</strong> and<br />

infiltrates it with <strong>adhesive</strong> monomers. 15 The strong<br />

versions <strong>of</strong> self-etch <strong>adhesive</strong>s can completely<br />

dissolve or disperse smear layers, forming thick<br />

hybrid layers in intact <strong>dentin</strong> that approach those<br />

Conclusion: The <strong>filled</strong> <strong>adhesive</strong> One-Step Plus did not show any beneficial effect than<br />

the un<strong>filled</strong> <strong>adhesive</strong> One-Step on the mTBS <strong>to</strong> <strong>dentin</strong> with <strong>to</strong>tal-etch and self-etch<br />

techniques. Irrespective from the <strong>adhesive</strong> type, self-etch technique revealed lower<br />

<strong>bond</strong> <strong>strength</strong>s than the <strong>to</strong>tal-etch technique.<br />

Q 2005 Elsevier Ltd. All rights reserved.<br />

achieved with conventional <strong>to</strong>tal-etch technique.<br />

Conversely, intermediate strong and mild versions<br />

incorporate smear layers as part <strong>of</strong> the <strong>bond</strong>ed<br />

interface, forming only thin hybrid layers. 16 Both<br />

<strong>to</strong>tal and self-etch approaches rely on the impregnation<br />

and polymerization <strong>of</strong> the monomers in<strong>to</strong><br />

the exposed collagen <strong>of</strong> the demineralized <strong>dentin</strong><br />

surfaces, creating a hybrid layer and the stabilization<br />

<strong>of</strong> the hybrid layer was established by the<br />

<strong>adhesive</strong>. 17 Recently, in comparison <strong>to</strong> the <strong>to</strong>taletch<br />

<strong>adhesive</strong>s two-step self-etch <strong>adhesive</strong>s are<br />

becoming increasingly popular, because <strong>of</strong> the<br />

reduced post-operative 18 and technique sensitivity.<br />

16 In addition <strong>to</strong> these, they are less likely<br />

<strong>to</strong> result in a discrepancy between the depth <strong>of</strong><br />

demineralization and the depth <strong>of</strong> resin infiltration<br />

19 since both processes occur simultaneously. 15<br />

Using <strong>to</strong>tal-etch systems, fillers incorporated in<br />

<strong>adhesive</strong> resins may increase the <strong>adhesive</strong> viscosity,<br />

resulting in a reduction in <strong>adhesive</strong> penetration<br />

in<strong>to</strong> the demineralized <strong>dentin</strong> and <strong>bond</strong>ing <strong>to</strong><br />

<strong>dentin</strong>. 20,21 There is however, less information on<br />

the effect <strong>of</strong> the <strong>filled</strong> <strong>adhesive</strong>s on the <strong>bond</strong>ing <strong>of</strong><br />

two-step self-etch systems <strong>to</strong> <strong>dentin</strong>.<br />

The purpose <strong>of</strong> this study was <strong>to</strong> evaluate the<br />

effect <strong>of</strong> a <strong>filled</strong> <strong>adhesive</strong> (One-Step Plus; Bisco)<br />

versus an un<strong>filled</strong> <strong>adhesive</strong> (One-Step; Bisco) on the<br />

microtensile <strong>bond</strong> <strong>strength</strong> (mTBS) <strong>to</strong> <strong>dentin</strong> using<br />

<strong>to</strong>tal-etch (Uni-etch; Bisco) and self-etch (Tyrian<br />

SPE; Bisco) techniques.<br />

Material and methods<br />

E. Can Say et al.<br />

The materials and their compositions used in this<br />

study are listed in Table 1. Twenty non-carious<br />

extracted human third molars, s<strong>to</strong>red in iso<strong>to</strong>nic<br />

saline with thymol crystals at 4 8C, were ground<br />

flat using 180-grit silicon carbide (SiC) abrasive<br />

paper under running water <strong>to</strong> expose occlusal<br />

<strong>dentin</strong>. After the superficial <strong>dentin</strong> surfaces were<br />

polished with 600-grit SiC <strong>to</strong> standardize the<br />

smear layer, the teeth were randomly assigned<br />

<strong>to</strong> four groups according <strong>to</strong> the type <strong>of</strong> <strong>adhesive</strong><br />

(One-Step Plus; One-Step) and technique (<strong>to</strong>taletch;<br />

self-etch) being used. Bonding procedures<br />

were performed according <strong>to</strong> the manufacturer’s


<strong>Microtensile</strong> <strong>bond</strong> <strong>strength</strong> <strong>of</strong> <strong>adhesive</strong> <strong>to</strong> <strong>dentin</strong> using self-etch and <strong>to</strong>tal-etch technique 285<br />

Table 1 Materials used in the study.<br />

Materials Composition Manufacturer<br />

One-Step Plus Bis-GMA, BPDM, HEMA, CQ, p-dimethylaminobenzoic acid<br />

(co-initia<strong>to</strong>r), ace<strong>to</strong>ne, 8.5% glass fillers<br />

Bisco Inc, USA<br />

One-Step Bis-GMA, BPDM, HEMA, ace<strong>to</strong>ne Bisco Inc, USA<br />

Tyrian SPE Primer A: thymol blue, ethanol, water<br />

Primer B: AMPS, BisMEP, TPO, ethanol<br />

Bisco Inc, USA<br />

Uni-etch 32% Phosphoric acid, BAC Bisco Inc, USA<br />

Clearfil AP-X Bis-GMA, TEGDMA, filler (Barium, SiO2) Kuraray Co, Japan<br />

BPDM, Biphenyl-dimethacrylate; HEMA, 2-hydroxyethyl-methacrylate; Bis-GMA, Bisphenyl-glysidyl-methacrylate; AMPS, 2-<br />

Acrylamido-2-methylpropanesulfonic acid; BisMEP, Bis(2-(methacryloyloxy)ethyl)phosphate; TEGDMA, Triethylene glycol-dimethacrylate<br />

TPO:2,4,6 (trimethylbenzoyldiphenylphosphine) oxide; BAC, Benzalkonium chloride.<br />

instructions and summarized in Table 2. Then a<br />

resin composite (Clearfil AP-X; Kuraray Medical<br />

Co, Ltd, Tokyo, Japan) was built up incrementally.<br />

Each <strong>of</strong> the three resin composite increments<br />

was light cured for 20 s using a light-curing<br />

unit (XL 3000, 3MESPE, St Paul MN, USA) with the<br />

intensity at 600 mW/cm 2 . Following s<strong>to</strong>rage in<br />

distilled water at 37 8C for 24 h, the <strong>bond</strong>ed<br />

specimens were serially sectioned in<strong>to</strong> 0.7 mmthick<br />

slabs using a low-speed diamond saw<br />

(Isomet; Buehler Ltd, Lake Bluff, IL 60044) and<br />

then trimmed with a superfine diamond bur <strong>to</strong><br />

form hour-glass shapes with approximately 1 mm 2<br />

cross-sectional areas (nZ20) using a digital<br />

micrometer.<br />

The specimens were attached <strong>to</strong> a table-<strong>to</strong>p<br />

material tester (EZ-test, Shimadzu Co, Kyo<strong>to</strong>,<br />

Japan) with a cyanoacrylate glue (Zapit, DVA,<br />

Anaheim, CA, USA) and subjected <strong>to</strong> microtensile<br />

testing at a crosshead speed <strong>of</strong> 1 mm/min until they<br />

fractured. All <strong>of</strong> the <strong>bond</strong>ed specimens were<br />

capable <strong>of</strong> being tested. In order <strong>to</strong> observe the<br />

failure modes, the de<strong>bond</strong>ed specimens were fixed<br />

for at least 8 h in 10% neutral buffered formalin,<br />

placed on stubs followed by room desiccation, gold<br />

sputter-coated and observed with a scanning<br />

electron microscopy (JXA-5400, JEOL, Tokyo,<br />

Japan). Failure modes were classified in<strong>to</strong> one <strong>of</strong><br />

four categories: <strong>adhesive</strong> if de<strong>bond</strong>ing occured<br />

between resin and <strong>dentin</strong>, mixed if it exhibited<br />

partially <strong>adhesive</strong>, partially cohesive failure in<br />

<strong>bond</strong>ing resin or in hybrid layer, or cohesive in<br />

resin or cohesive in <strong>dentin</strong>.<br />

Two-way ANOVA was performed <strong>to</strong> evaluate the<br />

effect <strong>of</strong> two experimental fac<strong>to</strong>rs: <strong>adhesive</strong> type<br />

and application technique, and the interaction <strong>of</strong><br />

these two fac<strong>to</strong>rs on mTBS. Multiple comparisons<br />

were performed by Tukey’s post hoc test at a<br />

significance level <strong>of</strong> 0.05 using a computer s<strong>of</strong>tware<br />

(SPSS 11, SPSS Inc Chicago IL). Failure modes <strong>of</strong> the<br />

specimens were analyzed using chi-square test.<br />

Scanning electron microscopy<br />

Four non-carious third molars (one per group)<br />

were used for SEM examination <strong>of</strong> the resin-<strong>dentin</strong><br />

interfaces after argon ion etching. The teeth were<br />

prepared in the same manner as the <strong>bond</strong>ing<br />

procedure and then sectioned longitudinally <strong>to</strong> the<br />

<strong>bond</strong>ing surface under running water using a lowspeed<br />

diamond saw (Isomet, Buehler Ltd, Lake<br />

Bluff IL, USA) and s<strong>to</strong>red for 24 h in neutral<br />

formalin. The specimens were then embedded in<br />

epoxy resin (Epon 815, NISSIN EM Co Ltd, Tokyo,<br />

Table 2 Bonding procedures.<br />

Groups Application procedures<br />

One-Step Plus <strong>to</strong>tal-etch Apply etchant for 15 s, rinse etchant, slightly dry, leaving moist, apply <strong>adhesive</strong><br />

in two coats, air dry <strong>adhesive</strong>, light cure <strong>adhesive</strong> for 10 s<br />

One-Step Plus self-etch Air dry <strong>dentin</strong> for 5 s, apply Tyrian SPE in two coats, air dry primer, apply <strong>adhesive</strong><br />

in two coats, air dry <strong>adhesive</strong>, light cure <strong>adhesive</strong> for 10 s<br />

One-Step <strong>to</strong>tal-etch Apply etchant for 15 s, rinse etchant, slightly dry, leaving moist, apply <strong>adhesive</strong><br />

in two coats, air dry <strong>adhesive</strong>, light cure <strong>adhesive</strong> for 10 s<br />

One-Step self-etch Air dry <strong>dentin</strong> for 5 s, apply Tyrian SPE in two coats, air dry primer, apply <strong>adhesive</strong><br />

in two coats, air dry <strong>adhesive</strong>, light cure <strong>adhesive</strong> for 10 s


286<br />

Table 3 Mean microtensile <strong>bond</strong> <strong>strength</strong> <strong>to</strong> <strong>dentin</strong> using One-Step Plus and One-Step <strong>adhesive</strong>s with <strong>to</strong>tal and<br />

self-etch technique.<br />

Type <strong>of</strong> <strong>adhesive</strong> Technique MeanGsd<br />

Filled (One-Step Plus) Total-etch 38.8G12.2 a (nZ20)<br />

Filled (One-Step Plus) Self-etch 22.4G4 b (nZ20)<br />

Un<strong>filled</strong> (One-Step) Total-etch 33.9G8.5 a (nZ20)<br />

Un<strong>filled</strong> (One-Step) Self-etch 26.4G7.5 b (nZ20)<br />

Different superscript letters indicate significant differences by two-way ANOVA and post hoc Tukey’s test (p!0.05).<br />

Japan) and polished using wet silicon carbide<br />

abrasive papers and diamond pastes <strong>of</strong> decreasing<br />

abrasiveness <strong>to</strong> 0,25 mm (DP-Paste, P, Streuers<br />

A/S, Copenhagen, Denmark). They were then<br />

subjected <strong>to</strong> argon ion etching (EIS-1E, Elionix<br />

Ltd, Tokyo, Japan) for 5 min with a constant<br />

voltage <strong>of</strong> 1 kV and ion current density <strong>of</strong><br />

0.2 mA/cm 2 , with the ion beam directed 908 <strong>to</strong><br />

the specimen surface, 22 gold-sputter coated and<br />

observed using a scanning electron microscope<br />

(JSM 5400; JEOL Ltd, Tokyo, Japan).<br />

Four additional non-carious third molars (one<br />

per group) were used for SEM examination <strong>of</strong> the<br />

resin-<strong>dentin</strong> interfaces <strong>to</strong> serial acid-base treatment<br />

resistance. The specimens were prepared as<br />

in the above mentioned manner and polished.<br />

They were then subjected <strong>to</strong> 10% phosphoric acid<br />

treatment for 3–5 s 23 followed by 5% sodium<br />

hypochloride immersion for 5 min. 24 After being<br />

extensively rinsed, the specimens were dried<br />

gold-sputter coated and observed using a scanning<br />

electron microscope (JSM 6335F; JEOL Ltd,<br />

Tokyo, Japan).<br />

Results<br />

Two-way ANOVA showed that the mTBS results<br />

(Table 3) were significantly influenced by the<br />

technique (pZ0.000) but not by the type <strong>of</strong><br />

<strong>adhesive</strong> (pZ0.836). The interaction <strong>of</strong> these two<br />

fac<strong>to</strong>rs was significant (pZ0.025), indicating that<br />

the differences that existed between two techniques<br />

(<strong>to</strong>tal-etch and self-etch) were not dependent<br />

on the type <strong>of</strong> <strong>adhesive</strong>.<br />

Multiple comparisons (post hoc Tukey’s test)<br />

revealed that <strong>to</strong>tal-etch technique exhibited significantly<br />

higher <strong>bond</strong> <strong>strength</strong> values than the selfetch<br />

technique with both <strong>filled</strong> (pZ0.000) and<br />

un<strong>filled</strong> <strong>adhesive</strong>s (pZ0.031). The mTBS <strong>of</strong> the <strong>filled</strong><br />

<strong>adhesive</strong> One-Step Plus (38.8G12.2 MPa) and the<br />

un<strong>filled</strong> <strong>adhesive</strong> One-Step (33.9G8.5 MPa) were<br />

not significantly different when they were used with<br />

the <strong>to</strong>tal etch (pZ0.298), and with the self-etch<br />

E. Can Say et al.<br />

technique (22.4G4.0 and 26.4G7.5 MPa, respectively)<br />

(pZ0.459).<br />

SEM observations <strong>of</strong> the resin-<strong>dentin</strong> interfaces<br />

revealed that the thickness <strong>of</strong> the hybrid layers<br />

Figure 1 (A) Scanning electron micrograph <strong>of</strong> the resin–<br />

<strong>dentin</strong> interface <strong>bond</strong>ed with One-Step Plus with <strong>to</strong>taletch<br />

technique after argon ion etching. Hybrid layer was<br />

3 mm thick. Fillers were uniformly dispersed in the<br />

<strong>adhesive</strong> layer and were evident around the tubuler<br />

orifices and in the tubules (arrow). c, composite; fa, <strong>filled</strong><br />

<strong>adhesive</strong>; h, hybrid layer; d, <strong>dentin</strong>. (B) Scanning electron<br />

micrograph <strong>of</strong> the resin–<strong>dentin</strong> interface <strong>bond</strong>ed with<br />

One-Step Plus with <strong>to</strong>tal-etch technique subjected <strong>to</strong><br />

sequential acid–base treatment. Hybrid layer was<br />

approximately 3 mm thick and resin-tags (arrow) penetrating<br />

in<strong>to</strong> <strong>dentin</strong>al tubules were clearly observed.<br />

Adhesive layer was 17 mm thick. c, composite; fa, <strong>filled</strong><br />

<strong>adhesive</strong>; h, hybrid layer; d, <strong>dentin</strong>.


<strong>Microtensile</strong> <strong>bond</strong> <strong>strength</strong> <strong>of</strong> <strong>adhesive</strong> <strong>to</strong> <strong>dentin</strong> using self-etch and <strong>to</strong>tal-etch technique 287<br />

Figure 2 (A) Scanning electron micrograph <strong>of</strong> the resin–<br />

<strong>dentin</strong> interface <strong>bond</strong>ed with One-Step Plus with selfetch<br />

technique after argon ion etching. Thickness <strong>of</strong> the<br />

hybrid layer (3.5 mm) was similar <strong>to</strong> the One-Step Plus<br />

<strong>to</strong>tal-etch group (Fig. 1(A) and (B)) and the <strong>adhesive</strong><br />

layer was 10 mm thick. c, composite; fa, <strong>filled</strong> <strong>adhesive</strong>;<br />

h, hybrid layer; d, <strong>dentin</strong>. (B) Scanning electron<br />

micrograph <strong>of</strong> the resin–<strong>dentin</strong> interface <strong>bond</strong>ed with<br />

One-Step Plus with self-etch technique subjected <strong>to</strong><br />

sequential acid–base treatment. Thickness <strong>of</strong> the hybrid<br />

layer (3.5 mm) and the <strong>adhesive</strong> layer (17 mm) were<br />

similar <strong>to</strong> the One-Step Plus <strong>to</strong>tal-etch group (Fig. 1(B)).<br />

Resin penetration in<strong>to</strong> <strong>dentin</strong>al tubules were observed<br />

(arrow) c, composite; fa, <strong>filled</strong> <strong>adhesive</strong>; h, hybrid layer;<br />

d, <strong>dentin</strong>; g, gap induced between hybrid layer and<br />

<strong>adhesive</strong>.<br />

created with the <strong>filled</strong> One-Step Plus and the<br />

un<strong>filled</strong> One-Step <strong>adhesive</strong>s using the <strong>to</strong>tal-etch<br />

technique were approximately 3 mm (Figs. 1(A) and<br />

(B), 3(A) and (B)), and when using self-etch<br />

technique, the hybrid layers <strong>of</strong> both <strong>adhesive</strong>s<br />

were also a similar thickness <strong>of</strong> 3.5 mm (Figs. 2(A)<br />

and (B), 4(A) and (B)). The <strong>adhesive</strong> layers achieved<br />

with the <strong>filled</strong> <strong>adhesive</strong> One-Step Plus both with<br />

<strong>to</strong>tal-etch and self-etch techniques were thicker<br />

(12–17 and 10–17 mm, respectively; Figs. 1(A) and<br />

(B), 2(A) and (B)) than the un<strong>filled</strong> <strong>adhesive</strong> One-<br />

Step (2 mm) (Figs. 3(A) and (B), 4(A)). Fillers were<br />

Figure 3 (A) Scanning electron micrograph <strong>of</strong> the resin–<br />

<strong>dentin</strong> interface <strong>bond</strong>ed with One-Step with <strong>to</strong>tal-etch<br />

technique after argon ion etching. The hybrid layer was<br />

3 mm thick and the <strong>adhesive</strong> layer was 2 mm thick.<br />

Adhesive layer (a) created with the un<strong>filled</strong> <strong>adhesive</strong><br />

was very thin (compare Fig. 1(A) and (B)). c, composite;<br />

h, hybrid layer; d, <strong>dentin</strong>. (B) Scanning electron<br />

micrograph <strong>of</strong> the resin–<strong>dentin</strong> interface <strong>bond</strong>ed with<br />

One-Step with <strong>to</strong>tal-etch technique subjected <strong>to</strong> sequential<br />

acid–base treatment. The hybrid layer was 3 mm thick<br />

and the <strong>adhesive</strong> layer was only 2 mm thick. Resin-tags<br />

(arrow) were penetrated deeply in<strong>to</strong> <strong>dentin</strong>al tubules.<br />

Adhesive layer (a) created with the un<strong>filled</strong> <strong>adhesive</strong><br />

was very thin (compare Fig. 1(A) and (B)). c, composite,<br />

h, hybrid layer, d, <strong>dentin</strong>.<br />

uniformly dispersed in the <strong>adhesive</strong> layers (Figs.<br />

1(A) and (B), 2(A)) and were evident around the<br />

tubular orifices and in<strong>to</strong> some <strong>dentin</strong> tubules<br />

(Fig. 1(A)) with the <strong>to</strong>tal-etch technique.<br />

Failure modes <strong>of</strong> the specimens in various<br />

groups are shown in Table 4. SEM <strong>of</strong> the<br />

representative de<strong>bond</strong>ed specimens are shown<br />

in Figs. 5–8. Chi-squared analysis revealed that<br />

One-Step Plus self-etch group, which provided<br />

the lowest mTBS among the all groups, was<br />

significantly different from the other groups<br />

(p!0.05) and 85% <strong>of</strong> the specimens showed


288<br />

Figure 4 (A) Scanning electron micrograph <strong>of</strong> the resin–<br />

<strong>dentin</strong> interface <strong>bond</strong>ed with One-Step with self-etch<br />

technique after argon ion etching. Thickness <strong>of</strong> the hybrid<br />

layer (3.5 mm) was similar <strong>to</strong> the One-Step <strong>to</strong>tal-etch<br />

group (Fig. 3(A) and (B)). The un<strong>filled</strong> <strong>adhesive</strong> layer was<br />

only 2 mm thick (compare Fig. 2(A) and (B)). c, composite;<br />

a, <strong>adhesive</strong>; h, hybrid layer; d, <strong>dentin</strong>. (B) Scanning<br />

electron micrograph <strong>of</strong> the resin–<strong>dentin</strong> interface <strong>bond</strong>ed<br />

with One-Step with self-etch technique subjected <strong>to</strong><br />

sequential acid–base treatment. Thickness <strong>of</strong> the hybrid<br />

layer (3.5 mm) was similar <strong>to</strong> the One-Step <strong>to</strong>tal-etch<br />

group (Fig. 3(A) and (B)). c, composite; a, <strong>adhesive</strong>; h,<br />

hybrid layer; d, <strong>dentin</strong>, g, gap induced in the <strong>adhesive</strong><br />

layer and between hybrid layer and <strong>adhesive</strong> layer.<br />

<strong>adhesive</strong> failures (Fig. 6). Using <strong>to</strong>tal-etch technique,<br />

the <strong>filled</strong> <strong>adhesive</strong> One-Step Plus (Fig. 5)<br />

and un<strong>filled</strong> <strong>adhesive</strong> One-Step (Fig. 7) showed<br />

mostly mixed failures.<br />

Discussion<br />

E. Can Say et al.<br />

Filled <strong>adhesive</strong>s were expected <strong>to</strong> act as an<br />

intermediate shock-absorbing elastic layer<br />

between composite resin and <strong>dentin</strong>, thus increasing<br />

the <strong>bond</strong> <strong>strength</strong> <strong>to</strong> <strong>dentin</strong>. 1,3,20 Many studies<br />

evaluated comparisons between commercially<br />

available <strong>filled</strong> and un<strong>filled</strong> <strong>adhesive</strong>s however,<br />

the advantages <strong>of</strong> these <strong>adhesive</strong>s as stress buffers<br />

remain unpredictable 7 and have not been substantiated<br />

with in vitro <strong>bond</strong> tests 25–29 and a clinical<br />

trial. 30 Filler type, size, shape, its surface characteristics,<br />

their interaction with the resin matrix and<br />

various solvents in the <strong>adhesive</strong>s may affect the<br />

<strong>bond</strong> <strong>strength</strong>. 20,21,31–33 The un<strong>filled</strong> <strong>adhesive</strong> One-<br />

Step and <strong>filled</strong> <strong>adhesive</strong> One-Step Plus, used in this<br />

study, utilizes ace<strong>to</strong>ne as a solvent. Besides, One-<br />

Step Plus consists <strong>of</strong> 8.5% Glass fillers with an<br />

average particle size <strong>of</strong> 1 mm. SEM observations <strong>of</strong><br />

the resin-<strong>dentin</strong> interfaces revealed that the<br />

thickness <strong>of</strong> the hybrid layer created with One-<br />

Step Plus was almost similar <strong>to</strong> that achieved with<br />

One-Step both with <strong>to</strong>tal-etch (approximately<br />

3 mm; Figs. 1(B) and 3(B), respectively) and selfetch<br />

(approximately 3.5 mm; Figs. 2(B) and 4(B))<br />

techniques. Conversely, the <strong>adhesive</strong> layer <strong>of</strong> the<br />

<strong>filled</strong> <strong>adhesive</strong> was thicker (Figs. 1(A) and (B), 2(A)<br />

and (B)) than the un<strong>filled</strong> <strong>adhesive</strong> (Fig. 3(A) and<br />

(B), 4(A)). Filler particles were found around the<br />

tubular orifices and in some <strong>dentin</strong> tubules<br />

(Fig. 1(A)) with the <strong>to</strong>tal-etch technique, however<br />

they were not capable <strong>of</strong> penetrating in<strong>to</strong> the<br />

spaces between collagen fibers because the width<br />

<strong>of</strong> interfibrillar spaces is about 20 nm. 9 The results<br />

<strong>of</strong> the microtensile <strong>bond</strong> test showed that <strong>bond</strong><br />

<strong>strength</strong>s <strong>to</strong> <strong>dentin</strong> between <strong>filled</strong> <strong>adhesive</strong> One-<br />

Step Plus and the un<strong>filled</strong> <strong>adhesive</strong> One-Step were<br />

not significantly different when they were used with<br />

the <strong>to</strong>tal etch (38.8G12.2 and 33.9G8.5 MPa,<br />

respectively) and with the self-etch technique<br />

(22.4G4.0 and 26.4G7.5 MPa, respectively).<br />

These results might indicate that the penetration<br />

ability <strong>of</strong> the resin monomer and the evaporation<br />

rate <strong>of</strong> water/solvent from <strong>dentin</strong> subsurface are<br />

not so different between <strong>filled</strong> and un<strong>filled</strong><br />

Table 4 Failure modes <strong>of</strong> the specimens after microtensile <strong>bond</strong> test.<br />

Groups Adhesive Mixed Cohesive in <strong>dentin</strong> Cohesive in composite<br />

One-Step Plus <strong>to</strong>tal-etch 3 15 2 –<br />

One-Step Plus self-etch 17 3 – –<br />

One-Step <strong>to</strong>tal-etch 5 15 – –<br />

One-Step self-etch 14 6 – –<br />

Adhesive, between resin and <strong>dentin</strong>; Mixed, partially <strong>adhesive</strong>, partially cohesive failure in <strong>bond</strong>ing resin or hybrid layer; Cohesive in<br />

<strong>dentin</strong>; Cohesive in resin.


<strong>Microtensile</strong> <strong>bond</strong> <strong>strength</strong> <strong>of</strong> <strong>adhesive</strong> <strong>to</strong> <strong>dentin</strong> using self-etch and <strong>to</strong>tal-etch technique 289<br />

Figure 5 Scanning electron micrograph <strong>of</strong> the fractured<br />

surface <strong>of</strong> One-Step Plus <strong>to</strong>tal-etch group showing<br />

mixed failure. d: cohesive in <strong>dentin</strong>, b: cohesive in<br />

<strong>bond</strong>ing resin, a: <strong>adhesive</strong> failure.<br />

<strong>adhesive</strong>s, although they have different viscosities<br />

because <strong>of</strong> the 8.5% filler load. Moreover, similar<br />

<strong>bond</strong> <strong>strength</strong>s <strong>to</strong> <strong>dentin</strong> may be due <strong>to</strong> the<br />

application <strong>of</strong> resin composites <strong>to</strong> a flat <strong>dentin</strong><br />

surface because the polymerization shrinkage <strong>of</strong><br />

the composite resin would minimize stress at the<br />

<strong>bond</strong>ed interface. 26<br />

Stress distribution during tensile testing<br />

between <strong>filled</strong> and un<strong>filled</strong> <strong>adhesive</strong>s has been<br />

expected <strong>to</strong> be different because <strong>adhesive</strong>s containing<br />

fillers showed higher elastic modulus than<br />

un<strong>filled</strong> resins. 25 However, the failure modes <strong>of</strong> the<br />

<strong>filled</strong> and un<strong>filled</strong> <strong>adhesive</strong>s with <strong>to</strong>tal-etch technique<br />

(Figs. 5 and 7, respectively) were similar<br />

Figure 6 Scanning electron micrograph <strong>of</strong> the fractured<br />

surface <strong>of</strong> One-Step Plus self-etch group showing<br />

<strong>adhesive</strong> failure.<br />

Figure 7 Scanning electron micrograph <strong>of</strong> the fractured<br />

surface <strong>of</strong> One-Step <strong>to</strong>tal-etch group showing<br />

mixed failure. a: <strong>adhesive</strong> failure, b: cohesive in <strong>bond</strong>ing<br />

resin.<br />

showing predominantly mixed failure (Figs. 5<br />

and 7, respectively) and also similar with the<br />

self-etch technique showing <strong>adhesive</strong> failure<br />

(Figs. 6 and 8, respectively). This may be due <strong>to</strong><br />

the fact that the application <strong>of</strong> a thin layer <strong>of</strong> a<br />

more flexible <strong>adhesive</strong> (lower elastic modulus)<br />

(Figs. 3(A) and 4(A)) led <strong>to</strong> the same stress relief as<br />

thick layers <strong>of</strong> a less flexible <strong>adhesive</strong> (higher<br />

elastic modulus) 34 (Figs. 1(A) and 2(A)).<br />

Self-etch <strong>adhesive</strong>s have been classified on their<br />

ability <strong>to</strong> penetrate smear layers and their depth <strong>of</strong><br />

demineralization in<strong>to</strong> the subsurface <strong>dentin</strong> as<br />

mild, intermediary strong and strong. 16,35 The<br />

self-etching primer Tyrian SPE used in this study<br />

Figure 8 Scanning electron micrograph <strong>of</strong> the fractured<br />

surface <strong>of</strong> One-Step self-etch group showing<br />

<strong>adhesive</strong> failure.


290<br />

can be considered as a strong self-etching primer<br />

because <strong>of</strong> its low pH, 1.0. 36 This high acidity<br />

results in deeper demineralization and the hybrid<br />

layer thickness using the self-etching primer Tyrian<br />

SPE resembled those <strong>of</strong> the <strong>to</strong>tal-etch technique<br />

both with <strong>filled</strong> and un<strong>filled</strong> <strong>adhesive</strong>s, whose<br />

thickness is different from the other self-etch<br />

primer/<strong>adhesive</strong> systems (i.e.: Clearfil SE Bond). 37<br />

However as previously reported hybrid layer thickness<br />

does not correlate with <strong>bond</strong> <strong>strength</strong> values 38<br />

and microtensile <strong>bond</strong> <strong>strength</strong>s <strong>to</strong> <strong>dentin</strong> in<br />

comparison <strong>to</strong> the <strong>to</strong>tal-etch technique was compromised<br />

when the self-etching primer Tyrian SPE<br />

was used (Table 3). In addition, the de<strong>bond</strong>ed<br />

specimens <strong>of</strong> the Tyrian SPE groups showed mainly<br />

<strong>adhesive</strong> failures (Figs. 6 and 8), whereas the <strong>to</strong>taletch<br />

specimens showed mostly mixed failures<br />

(Figs. 5 and 7). These lower <strong>bond</strong> <strong>strength</strong>s using<br />

Tyrian SPE both with <strong>filled</strong> and un<strong>filled</strong> <strong>adhesive</strong>s<br />

may be attributed <strong>to</strong> these fac<strong>to</strong>rs: Tyrian SPE<br />

contains a high concentration <strong>of</strong> ethanol and water.<br />

Although it would be desirable <strong>to</strong> remove all water<br />

and solvent at the end <strong>of</strong> the etching time, acidic<br />

monomers, dissolved calcium and phosphate ions<br />

may lower their vapor pressure. Residual water in<br />

the <strong>dentin</strong> subsurface may interfere with polymerization<br />

<strong>of</strong> the mixture <strong>of</strong> the self-etching primer<br />

and the <strong>adhesive</strong> resin, thereby lowering the quality<br />

<strong>of</strong> the hybrid layer. 39<br />

In addition <strong>to</strong> this, the problem may be further<br />

aggravated by the addition <strong>of</strong> One-Step Plus and<br />

One-Step, which also contains a high concentration<br />

<strong>of</strong> ace<strong>to</strong>ne. It has been shown that incomplete<br />

removal <strong>of</strong> ace<strong>to</strong>ne from the <strong>adhesive</strong> layer <strong>of</strong> twostep<br />

<strong>to</strong>tal-etch <strong>adhesive</strong>s resulted in poor polymerization<br />

<strong>of</strong> resin and crack formation in the<br />

<strong>adhesive</strong> layer or between <strong>adhesive</strong> and hybrid<br />

layer, leading <strong>to</strong> premature <strong>bond</strong> failure. 40–42 The<br />

observed gaps in One-Step Plus (Fig. 2(B)) and One-<br />

Step (Fig. 4(B)) self-etch groups may have been<br />

originated from or may have been increased by air<br />

drying and desiccating the specimens for SEM<br />

observation. However since such gaps or cracks<br />

were not evident in <strong>to</strong>tal-etch groups, and since all<br />

specimens were treated in the same manner, they<br />

may have been attributed <strong>to</strong> poorly polymerized<br />

hybrid/<strong>adhesive</strong> layers.<br />

In conclusion, the 8.5% glass-<strong>filled</strong> <strong>adhesive</strong> One-<br />

Step Plus did not show any beneficial effect than the<br />

un<strong>filled</strong> <strong>adhesive</strong> One-Step on the mTBS <strong>to</strong> <strong>dentin</strong><br />

with <strong>to</strong>tal-etch and self-etch techniques. Irrespective<br />

from the <strong>adhesive</strong> type, self-etch technique<br />

revealed lower <strong>bond</strong> <strong>strength</strong>s than the <strong>to</strong>tal-etch<br />

technique. Further research is necessary <strong>to</strong> compare<br />

the effects <strong>of</strong> fillers in <strong>adhesive</strong>s with the same resin<br />

composition and solvent on <strong>bond</strong>ing <strong>to</strong> <strong>dentin</strong> within<br />

various cavity shapes and on the durability <strong>of</strong> the<br />

resin-<strong>dentin</strong> <strong>bond</strong>s made with these <strong>adhesive</strong>s using<br />

<strong>to</strong>tal-etch and self-etch techniques.<br />

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