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Effect of Aging Conditions on the Repair Bond Strengthlication
t ot

n
of a Microhybrid and a Nanohybrid Resin Compositeesse nc e fo r

Mutlu Özcana/Cenk Curab/Johannes Brendekec

Purpose: This study evaluated the effect of different aging methods on the repair bond strength and failure types of a
microhybrid and a nanohybrid composite.
Materials and Methods: Disk-shaped microhybrid (Quadrant Anterior Shine-QA) and nanohybrid (Tetric EvoCeram-TE)
resin composite specimens (N = 192, n = 12/per group) were photopolymerized and randomly assigned to one of the
three aging conditions: (1) immersion in deionized water (37°C, 2 months), (2) thermocycling (5000 times, 5 to 55 °C), (3)
immersion in citric acid (pH: 3.0; 1 week). The control group was stored dry for 24 h at 37°C. After aging procedures,
the specimens were silica coated (30 μm SiO2) (CoJet-Sand) using an intraoral air abrasion device, silanized (ESPE-
Sil) and an intermediate adhesive resin was applied (Visio-Bond, 3M ESPE). Resin composites, once of the same kind
as the substrate (QA-QA, TE-TE) and once other than the substrate material (QA-TE, TE-QA) were adhered onto the con-
ditioned substrates. Shear force was applied to the adhesive interface in a universal testing machine (cross-head
speed: 1 mm/min).
Results: A significant influence of the aging method was observed (p < 0.05) but the composite type did not affect
the repair bond strength (p = 0.755) (2-way ANOVA, Tukey’s test). Interaction terms were significant (p < 0.05). Ther-
mocycling showed lower results (10 ± 2.6 to 14.4 ± 4.4 MPa) than those of other aging methods (12.7 ± 5.2 to 28 ±
5.3 MPa). Using the substrate and the adherend interchangeably (QA-TE, TE-QA) did not show significant differences
in the control group, but the results were significant after aging (p = 0.007) (2-way ANOVA, Tukey’s test). Interaction
terms were not significant (p = 0.124). The incidence of score A (cohesive failures in the substrate) was not signifi-
cant between the composite combinations in the control groups (exclusively 100%) and water-storage aged groups
(92% to 100%) (p > 0.05) (chi-square). Citric acid aging yielded significantly less incidence of score A (8-75%) com-
pared to the control group in all composite combinations (p < 0.05).
Conclusion: Both microhybrid and nanohybrid composites could be used either as a substrate or as relayering com-
posites in early repairs. Aging factors may diminish the repair quality.
Keywords: aging, microhybrid composite, nanohybrid composite, repair, silica coating, surface conditioning.

J Adhes Dent 2010; 12: 451-459. Submitted for publication: 22.09.09; accepted for publication: 01.10.09.
doi: 10.3290/j.jad.a17857

R esin-based composite materials (hereafter: compos-

ites) are widely used, especially in the field of restora-
a Professor, University of Zürich, Dental Materials Unit, Center for Dental and
Oral Medicine, Clinic for Fixed and Removable Prosthodontics and Dental
Materials Science, Zürich, Switzerland.
b Associate Professor, Ege University, Department of Prosthodontics, Izmir,
Turkey.
c Dental Student, University Medical Center Groningen, University of Gronin-
gen, Department of Dentistry and Dental Hygiene, Groningen, The Nether-
lands.
Correspondence: Prof. Dr. med. dent. Mutlu Özcan, University of Zürich, Head
of Dental Materials Unit, Center for Dental and Oral Medicine Clinic for Fixed
and Removable Prosthodontics and Dental Materials Science, Plattenstrasse
11, CH-8032, Zürich, Switzerland. Tel: +41-44-63 45600, Fax: +41-44-63
44305. e-mail: mutluozcan@hotmail.com or mutlu.ozcan@zzmk.uzh.ch
tive dentistry. However, failures of resin composite restora-
tions are still being reported in clinical studies as ranging
between 5% and 45% during an observation period of 5 to
17 years.5,13 Failure of a dental composite is often the re-
sult of degradation processes taking place within the poly-
meric matrix and the silanized filler particles of the
composite. These degradation mechanisms are complex
and could be due to wear, abrasion, fatigue, or enzymatic,
hydrolytic, acidic, or temperature-related breakdown.24,34
When a composite restoration fails as a result of discol-
oration, microleakage, ditching at the margins, delami-
nation or simply fracture, the restoration needs to be
repaired or replaced.7,12,21,28
Total replacement of the restoration is the most common
procedure experienced in daily clinical practice.21 However,
this approach may be regarded as overtreatment when large
portions of the restorations are clinically considered to be in-

Vol 12, No 6, 2010 451


Özcan et al
tact. Moreover, complete removal of a failed restoration
would generally entail removal of enamel and/or dentin
leading to more loss of sound dental tissues, that could
eventually result in weakening of the tooth or injuries to the
pulp. In such cases, repair actions would preserve the tooth,
as it is often difficult to remove a tooth-colored adhesive
restoration without removing an integral part of the tooth.
In general, adhesion between two composite layers is
achieved in the presence of an oxygen inhibited layer of un-
polymerized resin.10 As aged restorations do not contain an
unpolymerized surface layer, several methods have been
suggested to improve the composite-composite adhesion,
such as roughening, etching the substrate surface with
acidulated phosphate fluoride15 or hydrofluoric acid gel,26
air-borne particle abrasion,3,4,30 or using silanes and inter-
mediate adhesive resins.1,11,14,16,18,19,40
Although promising results were obtained in some of
these surface conditioning methods in earlier studies, the
tests were often performed on non-aged substrates where
the results could be considered optimistic and do not rep-
resent the real-life clinical situations. Furthermore, earlier
studies were often performed using the same type of com-
posite as both the substrate and the adherend materi-
al.1,3,4,11,14-16,18,19,29 When a composite restoration fails
and the patient has visited several dentists, it is not always
possible to find out which composite material was used and
under which conditions it was polymerized. In such situa-
tions, often dissimilar composite materials are adhered to
each other during repair.
While the size of the filler particles is around 8 to 30 μm
in hybrid composites and 0.7 to 3.6 μm in microhybrids,22,23
recently, nanofillers with sizes ranging from 5 to 100
nanometers have been developed.20 Due to the reduced di-
mension and wide size distribution of the particles, an in-
creased filler load can be achieved with the consequence of
reducing the polymerization shrinkage.2 However, it has
been reported that light scattering produced by the nano-
fillers may interfere negatively, resulting in a lower degree of
conversion than in the hybrid composites.2,20 When this is
the case, higher repair strength can be expected from such
materials due to possibly unreacted monomers on the sur-
face. On the other hand, from the chemical perspective, hy-
pothetically no difference could be expected when different
composites are used interchangeably as substrate and ad-
herend, since both types of materials contain methacrylate
groups in their monomer matrices with a similar function of
adhesion.38 Very little is known about the influence of aging
on the repair bond strength when different composite types
are adhered to each other.41
Aging conditions may result in decreased physical or me-
chanical properties of the composite, and these changes
may consequently affect surface properties and thus the ad-
hesion properties onto such materials.24,39 Therefore, the
objectives of this study were to evaluate the effect of differ-
ent aging methods on the repair bond strength of microhy-
brid-nanohybrid composite combinations and to analyze the
failure types. The null hypotheses tested were: 1) the use of
dissimilar composites would not affect the results and 2) ag-
ing conditions would decrease the repair strength.
452
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MATERIALS AND METHODS rP
by N
ub
Q ui
lica
The product name, manufacturer, chemical composition tio
this study are n
and batch numbers of the materials used int e
ot
n
s e n c eof
listed in Table 1. Experimental groups and snumber
fo r
specimens are schematically presented depending on the
composite-composite combinations and the aging condi-
tions in Fig 1.
A total of 192 disk-shaped specimens were fabricated by
placing unpolymerized microhybrid (n = 96) (Quadrant An-
terior Shine-QA) and nanohybrid resin composite (n = 96)
(Tetric EvoCeram-TE) incrementally into cylindrical undercut
cavities (diameter: 6 mm, thickness: 2 mm) that were pre-
pared in autopolymerized polymethylmethacrylate (PMMA)
(Autoplast, Candulor; Wangen, Switzerland) surrounded by a
PVC cylinder (3 specimens per cylinder). The unpolymerized
composites were packed into the cavities with a hand in-
strument and photopolymerized incrementally in layers of
not more than 2 mm using a halogen photopolymerization
unit (Demetron LC, SDS Kerr; Orange, CA, USA) for 40 s from
a constant distance of 2 mm from the surface. Light inten-
sity was 800 mW/cm2 verified by a radiometer after every
12 specimens (Demetron LC, Kerr).
The surface layer was covered by a translucent Mylar
strip (KerrHawe; Bioggio, Switzerland) in order to create a
smooth surface and to prevent the oxygen inhibition layer.
Aging Methods
The nanohybrid (n = 24) and the microhybrid (n = 24) com-
posite substrates were randomly divided into four groups
and subjected to one of the following aging methods: (1)
immersion in deionized water (37°C, 2 months), (2) ther-
mocycling (Willytec; Gräfelfing, Germany) (5000 times, 5°C
to 55°C, dwell time: 30 s, transfer time from one bath to
the other: 5 s) and (3) immersion in citric acid (pH: 3.0;
1 week). The control group was stored dry for 24 h at
37°C.
Surface Conditioning Method
The repair process was achieved using an intraoral air
abrasion device (Dento-PrepTM, RØNVIG; Daugaard, Den-
mark) filled with 30 μm alumina particles coated with
silica (CoJet-Sand, 3M ESPE) from a distance of appro-
ximately 10 mm at a pressure of 2.5 bars for 4 s. Follow-
ing surface conditioning, the remnants of sand particles
were gently air blown. The conditioned substrates were
then coated with a 3-methacryloxypropyltrimethoxysilane
coupling agent, γ-MPS (ESPE-Sil, 3M ESPE) and left to
react for 5 min. Finally, a bonding agent (Visio-Bond, 3M
ESPE) was applied with a microbrush, air thinned and pho-
topolymerized for 20 s.
In addition, after silica coating and gentle air blasting, the
surfaces of one specimen from both TE and QA were gold
sputtered and examined using a scanning electron micro-
scope (SEM) (JSM-5500, Jeol Instruments; Tokyo, Japan).
Repair Composite Application
After surface conditioning, the specimens from each
group were randomly divided further into two groups (n =
12). Resin composites, once of the same kind as the sub-
The Journal of Adhesive Dentistry
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Table 1 Product name, manufacturer, composition and batch number of the materials used in this studyfor

by N
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Product name Manufacturer Chemical composition Batch number
cat
ion
te ot

n
PMMA AutoPlast, Candulor; Polymethylmethacrylate F42028
ss e n c e fo r
Wangen, Switzerland

Tetric EvoCeram (TE) Ivoclar Vivadent; Schaan, Dimethacrylate-based monomers J10513

Liechtenstein (17-18% weight), barium glass, J04088
ytterbium trifluoride, mixed oxide
and prepolymer containing fillers
(82-83% weight), additives, catalysts,
stabilizers and pigments
(<1.0% weight). The particle size of
the inorganic fillers is between
40 nm and 3000 nm with a mean
particle size of 550 nm.

Quadrant Anterior Cavex; Haarlem, The Netherlands Methacrylate-based monomers 010100C

Shine (QA) 23.7 w%, silica, silicate glass and 010101C
fluoride containing fillers 75.6 w%,
polymerization catalysts 0.6 w%,
inorganic pigments 0.1 w%

CoJet-Sand 3M ESPE; Seefeld, Germany Aluminium trioxide particles coated 165092

with silica, particles size: 30 μm

ESPE-Sil 3M ESPE 3-methacryloxypropyltrimethoxysilane, 152745

ethanol

Visio-Bond 3M ESPE Dicyclopentyldimethylene diacrylate, 260950

2-propenoic acid,2-methyl,2-(2-hydro-
xylethyl) (3-methoxypropyl) (aminoP
ethyl ester)
KerrHawe Striproll KerrHawe; Bioggio, Switzerland Polyester 70501796

strate and once other than the substrate, were adhered
onto the conditioned substrates using translucent polyeth-
ylene molds (inner diameter of 3.6 mm; height 5 mm) and
photopolymerized. Bonding procedures were carried out in
accordance with the manufacturers’ instructions by the
same operator throughout the experiments. The compos-
ite was packed against the substrate incrementally with a
hand instrument and light polymerized in two layers of not
more than 2 mm. For easy retrieval of the composite stub
after polymerization, the mold was filled 1 mm below the
total height of the mold. Each layer was polymerized for 40
s from a distance of 2 mm. After polymerization, the poly-
ethylene molds were gently removed from the test speci-
mens.
Testing Procedure and Failure Analysis
Specimens were then mounted in the jig of the universal
testing machine (Zwick ROELL Z2.5 MA 18-1-3/7; Ulm,
Germany) and the shear force was applied using a shear-
ing blade having a 45-degree bevel at its tip until failure
occurred. The load was applied to the adhesive interface
as close as possible to the surface of the substrate at a
crosshead speed of 1.0 mm/min, and the stress-strain
curve was analyzed with a software program (TestXpert,
Zwick ROELL; Ulm, Germany). After debonding, digital pho-
tos (Nikon D1, Micro Nikon 60 lens; Tokyo, Japan) were
taken from the substrate surfaces and the failure sites
were examined by two calibrated operators (M.Ö., J.B.)
both visually and from digital photographs using a soft-
ware program at 20X magnification (CorelDRAW 9.0, Corel
Corporation and Coral; Ottowa, Canada). Types of failures
were categorized as A) cohesive in the substrate, B) adhe-
sive at the interface, C) cohesive in the adherend.
Statistical Analysis
Statistical analysis was performed using SPSS 11.0 soft-
ware for Windows (SPSS; Chicago, IL, USA). Bond strength
data (MPa) were submitted to two-way analysis of variance
(ANOVA) with the shear bond strength as the dependent
variable, and composite types (2 levels) and aging meth-
ods (4 levels) as independent variables. Multiple compar-
isons were made using Tukey’s HSD test. In order to
investigate the effect of interchangeable use of substrate-
adherend combinations (2 levels) and aging methods (4

Vol 12, No 6, 2010 453

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Substrate Aging Adherend lica
tio
te n
ot

n
Microhybrid (n = 12) ss e n c e
fo r
Control Nanohybrid (n = 12)
(n = 24)

Microhybrid (n = 12)
Water
(n = 24) Nanohybrid (n = 12)
Nanohybrid
(n = 96)
Thermo
(n = 24) Microhybrid (n = 12)

Nanohybrid (n = 12)
Citric acid
(n = 24)
Microhybrid (n = 12)

Nanohybrid (n = 12)
Specimen
(N = 192)
Microhybrid (n = 12)

Control Nanohybrid (n = 12)

(n = 24)

Microhybrid (n = 12)
Water
(n = 24) Nanohybrid (n = 12)
Microhybrid
( n = 96)
Thermo
(n = 24) Microhybrid (n = 12)

Nanohybrid (n = 12)
Citric acid
(n = 24)
Microhybrid (n = 12)
Fig 1 Schematic representation of
Nanohybrid (n = 12)
the experimental groups depending
on the composite-composite combina-
tions and the aging conditions.

Table 2a Results of 2-way ANOVA evaluating the effect of composite type and aging conditions on the repair strength

Source of variation Degree of freedom (df) Sum of squares (SS) Mean square (MS) Ratio (F) Probability (P)

Composite type 3 208.474 69.491 2.338 0.755

Aging type 3 2731.008 910.336 30.634 0.05*
Composite x aging 9 1191.915 132.435 4.457 0.05*
Error 171 5081.580 29.717
Total 187 64935.799

*Indicates significant effect on bond strength at α = 0.05.

levels) on the bond strength, a separate 2-way ANOVA and RESULTS

Tukey’s test were used. Furthermore, frequency of failure
types between groups was statistically analyzed using the The results of 2-way ANOVA are demonstrated in Tables 2a
chi-square test. P values less than 0.05 were considered and 2b. Mean values per group and significant differences
to be statistically significant in all tests. between the experimental groups are shown in Table 3.

454 The Journal of Adhesive Dentistry

 opyretigal
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Table 2b Results of 2-way ANOVA evaluating the effect of changing the substrate-adherend combinations andr aging

by N
conditions on the repair strength Pu
bli

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cat
Source of Degree of freedom (df) Sum of squares (SS) Mean square (MS) Ratio (F) Probability (P)
ion
te ot

n
variation ss e n c e fo r
Substrate- 1 186.126 186.126 7.537 0.007*
adherend
application
Aging type 3 1346.804 448.935 18.180 0.05*
Application x aging 3 145.959 48.653 1.970 0.124
Error 88 2173.116 24.695
Total 96 31516.609

*Indicates significant effect on bond strength at α = 0.05.

Table 3 The mean (± SD) bond strength values (MPa) for substrate-adherend combinations
with and without aging (control)

Control Water storage Thermocycling Citric acid Total

TE-QA 20.5 (6.5)A,a 19.2 (5.1)B,a 10.0 (2.6)D,b 12.7 (5.2)F,b 15.6 (6.6)
QA-QA 21.9 (10.0)A,c 18.3 (5.1)B,c 10.7 (4.5)D,d 18.7 (6.0)F,G,c 17.2 (7.6)
TE-TE 15.9 (4.7)A,f 28.0 (5.3)C,g 14.4 (4.4)E,f 12.9 (6.1)F,f 17.9 (8.0)
QA-TE 19.0 (5.6)A,h 23.6 (4.7)B,C,h 14.2 (3.7)E,i 16.7 (5.3)F,G,i 18.3 (5.9)
Total 19.4 (7.0) 22.3 (6.2) 12.3 (4.2) 15.2 (6.0) 17.2 (7.0)

Same upper-case letters represent no statistically significant difference within each column. Same lower-case letters
represent no statistically significant difference within each row compared to the control group (α = 0.05).

Fig 2a Representative specimen with cohesive failure in the sub- Fig 2b Representative specimen with adhesive failure at the in-
strate (score A). terface (score B).

A significant influence of the aging method was observed
(p < 0.05), but the composite type did not affect the repair
bond strength (p = 0.755) (2-way ANOVA, Tukey’s test). In-
teraction terms were significant (p < 0.05). While thermocy-
cled specimens showed lower results (10 ± 2.6 to 14.4 ± 4.4
MPa) than those of other aging methods (12.7 ± 5.2 to 28 ±
5.3 MPa), the repair strength of the water stored specimens
(18.3 ± 5.1 to 28 ± 5.3 MPa) were not significant when com-
pared to the control group (15.9 ± 4.7 to 21.9 ± 10) (p >
0.05).
Using the substrate and the adherend interchangeably
(QA-TE, TE-QA) did not show significant differences in bond
strength in the control group (p > 0.05) but the results were
significant after aging (p = 0.007) (2-way ANOVA, Tukey’s
test). Interaction terms were not significant (p = 0.124).
Among all aging conditions, after 2 months water storage,
the TE-TE combination (28 ± 5.3 MPa) showed the highest
mean bond strength followed by QA-TE (23.6 ± 4.7 MPa) (p
> 0.05).
Representative specimens from score A and score B fail-
ures are presented in Figs 2a and 2b. Table 4 shows the dis-

Vol 12, No 6, 2010 455

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Özcan et al
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Table 4 Distribution of failure types in percentage analyzed after bond strength test t fo
rP

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Q ui
Failure type Control Water aging Thermocycling Citric Acid Total lica
tio
ess c e n
t85 ot

n
TE-QA A 100a 92a 92a 55a,b fo r
B 0a 8a 8a 45b 15
en
C 0a 0a 0a 0a 0

QA-QA A 100a 100a 82b 75b 89

B 0a 0a 0a 25b 7
C 0a 0a 18b 0a 4

TE-TE A 100a 92a 92a 8b 72

B 0a 8a 8a 92b 28
C 0a 0a 0a 0a 0

QA-TE A 100a 92a 58b 42c 73

B 0a 8a 42b 58c 27
C 0a 0a 0a 0a 0

Total A 100 94 81 45 79
B 0 6 15 55 20
C 0 0 4 0 1

Score A: cohesive in the substrate; score B: adhesive at the interface; score C: cohesive in the adherend. The same superscript letters
in a row show no significant differences (chi-square test).

Fig 3a SEM image (10,000X) of typical silica coated surface of Fig 3b SEM image (10,000X) of typical silica coated surface of
TE. Note the presence of the attached silica particles even after QA. Note the presence of the attached silica particles even after
air blowing. air blowing.

tribution of failure types per experimental group. The inci- DISCUSSION

dence of score A (cohesive failures in the substrate) did not
differ significantly between the control group (100%) and wa-
ter-storage aged groups (92% to 100%) (p > 0.05) (chi-
square). Citric acid aging yielded significantly less incidence
of score A (8% to 75%) compared to the control group (ex-
clusively 100%) in all composite combinations (p < 0.05).
SEM analysis showed that after silica coating, both com-
posites presented deposits of sand particles even after air
blowing the remnants (Figs 3a and 3b).
This study was undertaken in order to evaluate the effect
of different aging methods and composite-composite com-
binations on the repair bond strength, employing the
shear bond strength test. In this kind of test, maximum
tensile forces and non-uniform stress distribution may
occur close to the cylinder-base interface.6,44 Furthermore,
surface tensile stresses are higher than interfacial vertical
tensile stresses, resulting in cohesive failures of the sub-

456 The Journal of Adhesive Dentistry


strate. The microtensile test, suggested by Sano et al,35
assesses the bond strength of specimens with reduced
areas of adhesive joint where fractures occur basically at
the adhesive interface. Although it can be true for the
dentin bonding studies,44 the results may differ with vary-
ing substrate materials.42 On the other hand, loading the
specimens under shear could be considered to be clini-
cally more relevant than those of flexural or tensile load-
ing, since it produces elements of shear, tensile and
compressive stresses that often occur during chewing
function. 37 Nevertheless, the results of each test me-
thod should be used for ranking purposes within each stu-
dy.8,42
In this study, the composite type, being either microhybrid
or nanohybrid, did not affect the repair bond strength sig-
nificantly, leading to rejection of the first hypothesis. After ag-
ing, the surfaces of all the specimens were conditioned us-
ing silica coating and silanization. Most probably, with the re-
pair method used, the substrate surface was coated evenly,
offsetting the variations in the surface composition of the
composites tested. This method, which comprises applica-
tion of air abrasion with 30 μm Al2O3 particles, modified with
silica (CoJet-Sand) was chosen based on previous favorable
findings4,25,26,29 over the other methods.3,4,26,29 Particle
deposition leads to a surface layer of a mixture of alumina
and silica particles.27 The surface is then coated with an
MPS silane that makes the surface more reactive for the
methacrylate groups of the repair resin. Particle deposition
techniques increase the surface area39,49 and at the same
time favor the surface wettability of the adhering resin or the
composite.25 SEM images clearly showed the deposits of the
sand particles on both composite types that act as sites for
the subsequently applied silane coupling agents. In the con-
trol group and after water storage, bond strength results and
the failure types – being almost exclusively cohesive in the
substrate (score A) – showed no significant differences be-
tween all substrate-adherend combinations, indicating that
early repairs with both microhybrid or nanohybrid compos-
ites are reliable.
After silica coating and silanization, according to the man-
ufacturer’s recommendations for this method, an interme-
diate adhesive resin (Visio-Bond) was used. Application of in-
termediate adhesive resin could result in swelling of the
monomer matrix of the substrate and create an interpene-
trating polymer network between the substrate and the ad-
herend, thereby improve the wettability.16 This diacrylate-
based intermediate adhesive was reported to have better
surface wetting properties compared to several other adhe-
sive resins.33 Different results could be expected when the
adhesive resins from the corresponding composite materi-
als are used in repair actions.
Although in the control group and water-stored group, the
mean bond strength results were comparable, a significant
effect of thermocycling and citric acid aging conditions was
noted on the repair strength. Since the interaction terms
were significant, the second hypothesis could only be par-
tially accepted. Among all aging methods tested, overall the
greatest decrease in bond strength was noted after thermo-
cycling compared to the control group. This was followed by
citric acid aging. In the oral environment, temperatures rang-
Vol 12, No 6, 2010
No CÖzcanopyretigal
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tf
ing between 5°C and 55°C are known to be theomostr P toler-
by N
ubde-
able temperatures.9 Such temperature alterations could
Q ui
lica
crease the number of unreacted double C=C bonds on the ti
te may af- on
surface or within the composite43 that consecutively
ot
n
ss e ninc ea
fo r
fect the composite-composite repair strength. Similarly,
previous study where a microtensile test was used,29 ther-
mocycling showed lower repair bond strength when com-
pared to the control group. Although mainly cohesive failures
in the substrate were found after thermocycling (58% to
92%), among all composite combinations after TC, only QA-
QA combinations showed cohesive failures in the adherend
(score C). One explanation for this could be the weaker co-
hesive strength of QA than the bond strength of the adhesive
joint.
Strong acids could disorganize the surface and dissolve
filler particles on the surface of a composite.15,26 While this
process increases microporosities on the surface due to
filler loss, it does not necessarily increase the adhesion of
resins to the etched surfaces, since penetration of the ad-
herend to the pores could not be guaranteed.15,26 The sig-
nificantly higher incidence of adhesive failures, indicating in-
sufficient repair strength in the citric-acid aged group com-
pared to the control group, supports this finding. Although
this may further indicate that acidic conditions may influ-
ence the double bonds,33,45 the amount of free radicals
may be less important due to the coating on the surface. In
order to make comparisons with previous studies,29,33,45
this medium was used to age the substrates. Although the
clinical relevance of exposure duration to citric acid (pH = 3,
1 week) could be questioned, exposing the speciments to
this medium may act as the accumulated effect of acidic
conditions or intake of beverages over time on composite
restorations. Further research is ongoing to investigate phys-
ical and chemical changes of the composite surfaces after
aging these conditions.33 Interestingly, the aging method of
water storage did not worsen the results when compared to
the control group. Even some increase in bond strength was
noted for TE-TE and QA-TE combinations. In fact, from water
storage for 2 months, some water diffusion into the sub-
strate could be expected.10,24 Two phenomena could be pre-
dicted to explain these results: either the aging effect was
not dramatic and therefore the surface free radicals were
not affected within the storage period and were sufficient for
good adhesion, or the surface softening through water led
to better penetration of the silica particles upon the impact
of the particles. Prolonged water storage requires further re-
search.
Although the bond strength required for a satisfactory
composite repair in vivo is not yet known, the bond strength
of composite to etched enamel is known to be in the range
of 15 to 30 MPa.17,36 Since composites on etched enamel
seldom fail mechanically, this range of bond strength could
be clinically considered as the golden standard. In the con-
trol group, and after 2 months of water storage, the obtained
results were higher than this range. However, some experi-
mental groups showed decreased bond strengths after ag-
ing conditions. It cannot be stated that the tested aging con-
ditions represent the worst-case scenario, but there was a
clear trend for the increase in adhesive failures indicating
that adhesion is in some ways impaired when the repair ac-
457

Özcan et al
tions are undertaken on aged composites. The increase in
adhesive failures at the interface (score B) after thermocy-
cling and the even greater increase after citric acid aging al-
so indicated a decrease in adhesion quality of the adhered
joints. This further indicates that not exlusively cohesive fail-
ures should be expected in the shear tests,6,44 and with the
decrease in adhesive strength, a trend to more adhesive fail-
ures was noted at least from the composite-comsposite com-
binations tested. Nevertheless, in judging the adhesive qual-
ity of repaired joints, both the bond strengths and the failure
types should be associated.
The attempt was made to simulate clinical situations in
which the practitioner is not able to identify the substrate
material to be repaired. For this reason, two different com-
posite materials were used interchangeably, QA and TE,
once as the substrate and the other time as the adherend.
This kind of application did not have a significant influence
on the bond strength in the control group, probably due to
sufficient free radicals available on the surface. This means
that when a restoration has failed, early repairs can be per-
formed using either a microhybrid or a nanohybrid compos-
ite. However, aging methods had a significant influence on
such substrate-adherend combinations.
In future studies, repair quality on polished composite
surfaces and the presence of the dental tissues surround-
ing the composite are warranted.
CONCLUSIONS
From this study, the following can be concluded:
1. The composite type, either microhybrid or nanohybrid,
did not have a significant effect on the repair bond
strength results with the repair method employed.
2. Repair bond strength after water storage did not de-
crease the bond strengths compared to the control
group, but aging the substrates with thermocycling or
citric acid did.
3. In the control group, exclusively cohesive failures were
observed in the substrate, but such failures were less
common after aging, and significantly less after citric
acid aging.
ACKNOWLEDGMENTS
The authors thank Mr. Ietse Stokroos for his assistance with the SEM
images. We also thank Cavex (The Netherlands) and Ivoclar Vivadent
(Liechtenstein) for supplying the composite materials.
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