d e n t a l m a t e r i a l s 2 3 ( 2 0 0 7 ) 1276–1282

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journal homepage: [Link]/journals/dema

Effect of surface conditioning methods on the

microtensile bond strength of resin composite
to composite after aging conditions

Mutlu Özcan a,∗ , Silvia Helena Barbosa b , Renata Marques Melo b ,

Graziela Ávila Prado Galhano b , Marco Antonio Bottino b
a University Medical Center Groningen, University of Groningen, Department of Dentistry and Dental Hygiene,
Clinical Dental Biomaterials, Antonius Deusinglaan 1, 9713 AV Groningen, The Netherlands
b São Paulo State University, Department of Dental Materials and Prosthodontics, São José dos Campos, Brazil

a r t i c l e i n f o a b s t r a c t

Article history: Objectives. This study evaluated the effect of two different surface conditioning methods
Received 21 July 2006 on the repair bond strength of a bis-GMA-adduct/bis-EMA/TEGDMA based resin composite
Accepted 16 November 2006 after three aging conditions.
Methods. Thirty-six composite resin blocks (Esthet X, Dentsply) were prepared
(5 mm × 6 mm × 6 mm) and randomly assigned into three groups for aging process: (a)
Keywords: immersion in citric acid (pH 3.0 at 37 ◦ C, 1 week) (CA); (b) boiling in water for 8 h (BW)
Aging process and (c) thermocycling (×5000, 5–55 ◦ C, dwell time: 30 s) (TC). After aging, the blocks were
Repair assigned to one of the following surface conditioning methods: (1) silica coating (30 ␮m
Resin composite SiOx ) (CoJet, 3M ESPE) + silane (ESPE-Sil) (CJ), (2) phosphoric acid + adhesive resin (Single
Surface conditioning Bond, 3M ESPE) (PA). Resin composite (Esthet·X® ) was bonded to the conditioned substrates
Silica coating incrementally and light polymerized. The experimental groups formed were as follows:
Gr1:CA + PA; Gr2:CA + CJ; Gr3:BW + PA; Gr4: BW + CJ; Gr5:TC + PA; Gr6: TC + CJ. The specimens
were sectioned in two axes (x and y) with a diamond disc under coolant irrigation in order to
obtain non-trimmed bar specimens (sticks, 10 mm × 1 mm × 1 mm) with 1 mm2 of bonding
area. The microtensile test was accomplished in a universal testing machine (crosshead
speed: 0.5 mm min−1 ).
Results. The means and standard deviations of bond strength (MPa ± S.D.) per group were as
follows: Gr1: 25.5 ± 10.3; Gr2: 46.3 ± 10.1; Gr3: 21.7 ± 7.1; Gr4: 52.3 ± 15.1; Gr5: 16.1 ± 5.1; Gr6,
49.6 ± 13.5. The silica coated groups showed significantly higher mean bond values after all
three aging conditions (p < 0.0001) (two-way ANOVA and Tukey tests, ˛ = 0.05). The interaction
effect revealed significant influence of TC aging on both silica coated and acid etched groups
compared to the other aging methods (p < 0.032). Citric acid was the least aggressive aging
medium.
Significance. Chairside silica coating and silanization provided higher resin–resin bond
strength values compared to acid etching with phosphoric acid followed by adhesive resin
applications. Thermocycling the composite substrates resulted in the lowest repair bond
strength compared to citric acid challenge or boiling in water.
© 2006 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

∗
Corresponding author. Tel.: +31 50 363 8528; fax: +31 50 363 2696.
E-mail address: mutluozcan@[Link] (M. Özcan).
0109-5641/$ – see front matter © 2006 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.
doi:10.1016/[Link].2006.11.007
 d e n t a l m a t e r i a l s 2 3 ( 2 0 0 7 ) 1276–1282 1277

however, this system has not been tried on aged compos-

1. Introduction ites.
Replacement or relayering due to discoloration, wear or
Resin-based composites (hereon = composites) are widely chipping of composites in restorative dentistry is often per-
employed in dentistry since the advent of adhesive technolo- formed after certain period of clinical service. Therefore, the
gies. Commercially available composites in the dental market age of the restoration to be repaired plays a fundamental role
are often composed of monomeric resin matrix, silanized in the bond strength of composite repairs [6,21]. Storage of
inorganic particles, polymerization initiators, inhibitors for the composite specimens in aqueous media at different peri-
storage stability and pigmentation for shading. Even though ods, thermocycling and surface polishing are some methods
the properties of composites have been enhanced, factors used to simulate the aging process of composite materials
such as wear, discoloration, polymerization shrinkage and in vitro [21,22]. The aging process attempts to reproduce the
microleakage still limit the longevity of composite restorations hydrolytic degradation occurring in the resin matrix and the
[1–3]. Composites may suffer from chemical degradation and silane coated inorganic fillers that occur in the conditions of
erosion depending on the composition of monomers, poly- oral environment.
merization of the matrix, degree of conversion and the oral Even though the literature presents several comparative
environment [4,5]. studies, there is no consensus as to the best surface treat-
Total replacement of the restoration is the most common ment for optimum repair strength of composites. Moreover,
procedure experienced in daily clinical practice [2]. However aging of the substrate has often not been considered in
this approach may be regarded as over-treatment since in previous studies. Therefore, the objective of this study was
most cases, large portions of the restorations may clinically to evaluate the effect of composite repair methods using
and radiographically be considered free of failures. More- two different surface conditioning methods after three aging
over, complete removal of the restoration inevitably results in conditions.
weakening of the tooth, unnecessary removal of intact dental
tissues and repeated injuries to the pulp [1]. By repair of com-
posite restorations, in the way of partial replacement of the 2. Materials and methods
restorative material, intact of part of the restoration and/or
tooth tissues could be maintained. Thirty-six composite blocks with dimensions of 5 mm × 6 mm
Studies on the repair of composites report a consider- × 6 mm were obtained with a micromatrix hybrid composite
able difficulty to establish a long lasting bonding between the with barium boron fluoroalumino silicate glass filler parti-
polymerized composite and fresh repair resin [6,7]. While in cles based on bis-GMA-adduct/bis-EMA/TEGDMA (Esthet·X® ,
previous studies, it was stated that 40–50% of the unreactive Dentsply, Milford, DE) according to the manufacturer’s instruc-
methacrylate groups are present after light polymerization tions, using a silicone matrix (Zetaplus, Zhermack, Badia
of the composites that allow for adhesion of new resin lay- Polesine, Italy). The composite was packed into the silicone
ers [8,9], others reported that unreactive methacrylate groups matrix using hand instruments and light polymerized (Ultra-
are reduced with time, thereby reducing the potential for Lume® LED 5, Ultradent, South Jordan, Utah).
bonding of resins [10,11]. Moreover, the intervention of instru- One surface of each composite block (6 mm × 6 mm) was
ments for polishing composites accelerates the reduction planed and polished in a machine using silicone carbide
of reactive groups and exposes the inorganic filler parti- papers with 1200-grit under cooling (3M, St. Paul, USA). All
cles to the surface that may not present further bonding blocks were ultrasonically cleaned (Vitasonic, Vita Zanhfab-
ability [8]. Some other studies have demonstrated that the rik, Germany) for 10 min using distilled water. The composite
composite–composite repair strengths could reach 20–80% of blocks were then randomly divided into three groups (n = 12),
the initial bond strength, considering the cohesive resistance according to the aging procedure: (a) immersion in citric acid
of the material [8,12,13]. (pH: 3.5 at 37 ◦ C, 1 week) (CA), (b) boiling in water for 8 h (BW)
A great variety of surface conditioning methods and and (c) thermocycling (5000 cycles, between 5 and 55 ◦ C, dwell
adhesion promoters have been proposed to improve the time: 30 s) (TC).
repair strength of composites, such as roughening with burs, After aging, the blocks were further subdivided into two
acid etching with hydrofluoric or phosphoric acid, air-borne groups (n = 6), depending on the surface conditioning method
particle abrasion with aluminium oxide with or without prior to repair.
silane coupling agents and resin based adhesive systems
[11]. It was also reported that acid etching of the surface 2.1. Surface conditioning methods and repair
does not increase or reduce the bond strength of repairs procedures
[11,14]. In several studies, airborne particle abrasion using
aluminium oxide particles led to significant increase in Silica coating (CJ): Chairside tribochemical silica coating was
the strength of composite repairs [15,16]. One other parti- achieved using an intraoral air abrasion device (Dento-PrepTM ,
cle abrasion method, tribochemical pretreatment, with the RØNVIG A/S, Daugaard, Denmark) filled with CoJet® -Sand
use of silica coated alumina particles was initially intro- (30 ␮m SiOx particles) (3 M ESPE, Seefeld, Germany) from a
duced for bonding composites to ceramic and metal surfaces distance of approximately 10 mm at a pressure of 2.5 bar for
[17–19]. This surface treatment using silica coating and 4 s. Following surface conditioning, the remnants of sand
silanization has been investigated for composite repairs particles were gently air blown, the conditioned substrates
of fresh composites [7,20]. As to the authors’ knowledge were coated with a 3-methacryloxypropyltrimethoxysilane
1278 d e n t a l m a t e r i a l s 2 3 ( 2 0 0 7 ) 1276–1282

coupling agent, ␥-MPS (ESPE-Sil, 3M ESPE) and a period of 5 min Pinhais, Brazil), as parallel as possible in relation to application
was allowed for its reaction. of the tensile load, and testing was performed at a cross speed
of 0.5 mm min−1 .
2.2. Phosphoric acid-adhesive resin (PA) The bond strength was calculated according to the formula
R = F/A, where “R” is the strength (MPa), “F” the load required
The substrates were etched with 35% phosphoric acid gel for rupture of the specimen and “A” is the interface area of
(Scotchbond Phosphoric Etchant, 3 M ESPE) for 1 min, rinsed the specimen (mm2 ), measured with a digital caliper before
and dried thoroughly. Then an intermediate monomer resin the test.
(Single Bond, 3M ESPE) was applied a thin layer, the solvent
was gently removed under compressed air and the resin was 2.5. Statistical analysis
light polymerized for 10 s according to the manufacturer’s
instructions. Statistical analysis was performed using the software Statis-
Resin composite (Esthet X® ) was then bonded to the condi- tix 8.0 for Windows (Analytical Software Inc., Tallahassee, FL,
tioned substrates incrementally using hand instruments and USA). Bond strength data (MPa) were submitted to analysis of
light polymerized until a height of 5 mm was achieved. variance (two-way ANOVA) considering the composite block
The coding for the experimental groups formed were as within the experimental conditions a random effect. Mul-
follows: Gr1:CA + PA; Gr2:CA + CJ; Gr3:BW + PA; Gr4: BW + CJ; tiple comparisons were made with Tukey’s adjustment test
Gr5:TC + PA; Gr6: TC + CJ. (˛ = 0.05) with the two surface conditioning methods and three
aging procedures as the independent factors. p-Values less
2.3. Specimen preparation for the microtensile test than 0.05 are considered to be statistically significant in all
tests.
Composite–composite blocks were sectioned using a diamond
disc (Microdont, São Paulo, Brazil, n. 34570) at low-speed,
3. Results
under water cooling, in a sectioning machine. Initially, the
composite blocks were fixated with cyanoacrylate adhesive gel
Significant interaction effect between aging conditions and
(Super Bonder Gel, Loctite Ltd., São Paulo, Brazil) on a metallic
surface conditioning methods were observed on the repair
base that was attached to the sectioning machine. The blocks
bond strength (two-way ANOVA, p < 0.05). Table 1 and Fig. 1
were positioned as perpendicular as possible in relation to the
display the mean microtensile bond strength and standard
diamond disc of the machine. The first section, measuring
deviations associated with the aging processes and surface
approximately 1 mm was discarded in case of the possibility
conditioning methods. Results of two-way analysis of variance
of excess or absence of composite at the interface that might
are demonstrated in Table 2.
alter the results. This process was followed for the other two
Aging the composite substrates with TC affected the repair
sections and thus only the central specimens were used for
bond strengths significantly in both surface conditioning
the experiments. Six stick specimen (sp) were obtained from
groups (CJ: 49.6 ± 13.5 and PA: 16.1 ± 5.1 MPa) compared to
each block. The sps had non-machined (non-trimmed) adhe-
the CA and BW aging methods (46.3 ± 10.1 and 21.7 ± 7.1 MPa,
sive zones with bonded area measuring approximately 1 mm2
respectively) (p < 0.032). After all three aging conditions, sil-
and 10 mm length. The sps were stored in water at 37 ◦ C for
ica coated and silanized groups showed significantly higher
24 h prior to tests.
bond values (46.3 ± 10.1 to 52.3 ± 15.1 MPa) compared to acid
etching with phosphoric acid and bonding agent applications
2.4. Microtensile bond strength test
(16.1 ± 5.1 to 25.5 ± 10.3 MPa) (p < 0.0001).

Each sp was fixated with cyanoacrylate gel (Super Bonder Gel,

Loctite Ltd., São Paulo, Brazil), keeping the adhesive zone free, 4. Discussion
to the rods of a device adapted for this test. The specimens
were positioned parallel to the long axis of the device in order Relayering failed composite restorations could be considered
to reduce the bending stresses. The device was fixated in the as a minimal invasive and cost-effective treatment option
universal testing machine (EMIC DL-1000, EMIC, São José dos in an attempt to prolong the service life of aged composite

Table 1 – Means and standard deviations (M ± S.D.) of the microtensile bond strength data (MPa) of the studied groups
Aging process Surface conditioning Row

Silica coating and silanization Phosphoric acid and adhesive resin

Citric acid 46.3 ± 10.1 a 25.5 ± 10.3 b 35.9 ± 14.6

Boiling in water 52.3 ± 15.1 a 21.7 ± 7.1 b,c 37.0 ± 19.4
Thermocycling 49.5 ± 13.5 a 16.1 ± 5.1 c 32.8 ± 19.6
Column 49.4 ± 13.2 21.1 ± 8.6

Same letters indicate no significant differences (Tukey’s test, ˛ = 0.05).

 d e n t a l m a t e r i a l s 2 3 ( 2 0 0 7 ) 1276–1282 1279

the surface area. Moreover, these retentive surface textures

favor the surface wettability that allows optimal adaptation
of the composite [6,23].
Chairside tribochemical silica coating system used in the
present study, resulted in the highest mean repair bond
strength values (49–52 MPa) regardless of the composite aging
method when compared with phosphoric acid and adhe-
sive resin application (16–25 MPa). Silica coating comprises air
abrasion with 30 ␮m Al2 O3 particles that are modified with
silica (CoJet-Sand) that leads to deposition of a mixture of alu-
mina and silica particles on the surface [18,28]. The surface is
then coated with silane that makes the surface more reactive
for the methacrylate groups of the repair resin. In the study of
Frankenberger et al. [7], fatigue resistance of the repaired resin
Fig. 1 – The mean microtensile bond strength values (MPa) after utilization of silica coating or carbide burs gave similar
for two surface conditioning methods and aging conditions results but Bouschlicher et al. [29] reported better outcomes
in boxplots. Horizontal line in middle of each boxplot with utilization of the CoJet-Sand compared to other repair
shows mean value; horizontal lines in the box give 25% and methods. It could be due to the fact that the former study did
75% quartiles; lines outside box give 5% and 95% quartiles. not employ silane coupling agent that might have impaired
the performance of this surface treatment method since silane
application is a crucial step in silica coating. Similarly, even
restorations. This study was undertaken in order to study the though some studies did not find any significant difference in
effect of aging and conditioning methods on repair strength repair bond strength of composites with or without the use of
of fresh composites to aged ones employing microtensile test. silane [29,30], others observed an increase in bond strength
Similar studies with the same objective, but on fresh compos- with utilization of silane [6,14,31]. According to Söderholm
ites, have utilized shear test with various adhesive promoters [6], wear of composite surface exposes silane-free inorganic
or composites [11,14,20,23]. However, shear test is not an ideal filler particles that impair chemical bonding to the new com-
mechanical test since it often leads to non-uniform distribu- posite layers. After storing the specimens for 6 months in
tion of the stresses at the adhesive area. In this kind of test, water, the author observed that specimens repaired using
maximum tensile forces occur close to load application area silane presented the same flexural strength compared to orig-
thereby affect the substrate more than the adhesive interface inal specimens, i.e. the same cohesive strength. Hisamatsu
itself [24,25]. The microtensile test, suggested by Sano et al. et al. [31] also found similar values of cohesive strength when
[26], assesses the bond strength of specimens with reduced silanes were associated in the repair procedure of composites.
areas of adhesive joint where fractures occur basically at the In this study, after conditioning the surface with silica
adhesive interface. For these reasons, in this study a microten- modified aluminium oxide particles ␥-MPS silane was applied
sile test was used. on the resin surface. Silanes are molecules with two func-
The surface conditioning methods indicated for composite tional groups: silanol groups react with the inorganic filler
repairs are often based on mechanical roughening with burs, particles of resin and organofunctional group reacts with the
airborne particle abrasion or simply using etching agents and methacrylate groups in the adhesive system. After finishing
adhesive systems [27]. Among the particle abrasion systems, and polishing procedures and aging due to the conditions
aluminium oxide has presented the best bond strength values in the oral environment, degradation of the silane layer sur-
compared to other methods since it yields to microretentions rounding the fillers may be expected. However, a covalent
on the composite surface [11,14,16]. Particle deposition, at bond may again be established between the monomers in
the same time, increases the ability of the new composite to the adhesive system and the inorganic filler particles in
mechanically interlock to the substrate due to the increase in the composite using the silanes. The silica present on the

Table 2 – Results of two-way analysis of variance for the experimental conditions

Source of variation d.f. SS MS F P

Replicas 5 29.3 5.9

Blocks 5 1807.4 361.5
Replicas × blocks 25 2241.2 89.6
Aging 2 676.1 338.1 2.92 0.0568
Thermocycling 1 43134.9 43134.9 371.98 0.0000*
Aging × thermocycling 2 1577.7 788.9 6.80 0.0014*
Error 175 20293.1 116.0

Total 2159 69759.7

∗
p < 0.05
1280 d e n t a l m a t e r i a l s 2 3 ( 2 0 0 7 ) 1276–1282

composite surface on the other hand, forms covalent bonds procedures in these studies, results ranged from 30 to 82%
between hydroxyl groups and silanol groups in the silane. The of the cohesive strength. The decrease in repair strength
methacrylate groups of the organosilane ␥-MPS compound was attributed to the accelerated reduction in unreacted
form covalent bonds with the repair resin when polymer- methacrylate groups with time and intervention of the instru-
ized. Moreover, the silane also increases the wettability of ments for polishing of composites [8]. According to Øysaed et
the adhesive system that could more easily infiltrate into the al. [37], residual monomers are the main components released
irregularities created by air abrasion. This could be one of the from composites after polymerization during the first 7 days,
reasons why superior results were obtained with this surface leading to a reduction in cross-linking.
conditioning system compared to phosphoric acid etching and Unfortunately, in ex vivo conditions it is almost impossible
adhesive application. to find a standardized simulation method for aging of com-
The use of phosphoric acid in fact does not necessitate posites. Among the aging methods studied, the acidic medium
the purchase of additional armamentarium in dental prac- decreased the bond strength the least and thermocycling the
tice such as chairside air abrasion devices making repairs most. Chemical degradation, may result in decreased physico-
cost-effective for the practitioners. However in this study, mechanical properties of the composite such as decreased
phosphoric acid application did not reveal increased repair diametral tensile strength, fracture toughness and hardness
strength in any of the aged groups compared to silica coating [38], or increase in wear [39] depending on the chemical com-
and silanization. Although the test methodologies are differ- position of the composite. Storage in citric acid for example
ent, this finding is in agreement with those of other studies is expected to provoke acidic degradation and thermocy-
[10,32]. Even though in the investigation of César et al. [33], cling and immersion in boiling water accelerate thermal and
the authors microscopically observed that phosphoric acid did hydrolytic degradation in the composite. Immersion in boiling
not alter the surface characteristics, Kula et al. [34] examined water or long term acid challenge, although not likely to occur
decomposition of the inorganic filler particles after immersion in the oral cavity, are considered as worst-case scenarios, to
of the composite in acidic medium. This decomposition may create combined effect of hydrolytic and thermal breakdown
impair the adhesion between composite layers but no differ- and to simulate accelarated aging [22]. Degradation of com-
ence was observed between utilization of acid alone or acid posites through acidic challenges is not widely studied but it
followed by adhesive in the study of César et al. [33], with is known that strong acids could dissolve filler particles on
results ranging from 20 to 22 MPa. Sau et al. [9] on the contrary, the surface of a composite [40]. While this process increases
found shear strength values ranging between 3 and 11 MPa. microporosities on the surface due to filler loss, it does not
The results presented in the aforementioned studies corrobo- necessarily increase the adhesion of resins to etched surfaces
rate the values found in the present study that ranged from 16 [40]. In this study, citric acid (pH 3.0) seemed to age the com-
to 25 MPa for the groups repaired using phosphoric acid and posite substrates less than thermocyling resulting in higher
the adhesive resin. To date clinically sufficient bond strength repair strengths.
is not known. Aiming for higher bond strength data could per- Water absorption effect in either boiling or thermocycling
haps be thought unnecessary however it should also be noted aging conditions has a deleterious effect on the structural
that higher repair bond strength and thereby good surface wet- and physical integrity of composites including flexural and
tening of the repair resin on the substrate would also decrease repair strength [41] due to hydrolytic degradation that occurs
the microleakage between the repaired layers that is often one by the process of oxidation and/or hydrolysis. The progressive
of the reasons why composite restorations need to be replaced. degradation of the microstructure occurs by the formation of
It could also be expected that utilization of intermediate pores, in which oligomers, residual monomers, products of
adhesive monomers would increase the repair bond stregth degradation and additives may be released [4,5]. The study
as reported earlier [16,23,35]. Adhesive promoters allow pen- of Ortengren et al. [5] revealed that TEGDMA was the most
etration of monomers into the roughened composite surface, released monomer. Hydrolytic degradation also promotes
creating a non-polymerized layer by inhibition of oxygen that leaching of quartz and silicon besides yielding cracks in the
would eventually aid adhesion of new composite layers. Inter- matrix [8]. When polymerized, the dental monomers often
mediate adhesive resins have also affinity to inorganic filler have incomplete double bond conversion [42]. As the poly-
particles through bonding to hydrogen and silane [23]. Investi- merization progresses, the network formation decrease the
gations evaluating the influence of different adhesive systems mobility of monomers and oligomeric molecules resulting
commercially available for composite repair, presented vari- in pendant methacrylate groups and unreacted monomer
ations in bond strength values depending on the adhesive trapped in the material. Low levels of conversion also affect
type [10,36]. Again, these studies were conducted on non-aged physical properties of the polymer, decreasing its strength.
composites. The amount of leached monomers out of the polymer may
When a resin layer is adhered to the other immediately vary with the type of monomers in the system. For the bis-
after light polymerization, bonding between the two lay- GMA containing polymers, the conversion degree ranges from
ers occurs due to inhibition of surface polymerization by 54 to 85% [42]. The composite used in our study is based on
the presence of oxygen that allows adhesion of unreacted bis-GMA/TEGDMA. The monomer leached from the polymer
methacrylate groups in the dispersion layer to the new incre- matrix is inversely correlated to the amount of TEGDMA in the
ment of resin. The adhesive strength between the resin system and positively correlated to base monomer concentra-
layers is considered as the cohesive strength of the material tion [43]. The results therefore may be affected when other
[6,10,11,14]. Comparison of the cohesive strength of compos- composites are used with such as UDMA/TEGDMA matrix or
ites with the repair strength of these materials after aging when dissimilar composites are adhered to one another.
 d e n t a l m a t e r i a l s 2 3 ( 2 0 0 7 ) 1276–1282 1281

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