Shear Bond Strength of Self-etching Bonding Systems

in Combination with Various Composites Used for

Repairing Aged Composites
Erica C. Teixeiraa/Stephen C. Bayneb/Jeffrey Y. Thompsonc/Andre V. Ritterd/Edward J. Swifte

Purpose: Repair of worn, broken or discolored composite restorations can be accomplished using new composite
material and dentin bonding systems. The purpose of this study was to investigate the effectiveness of self-etching
adhesive systems for composite re-bonding procedures onto different composite substrates that had been aged
for 6 years prior to testing.

Materials and Methods: Two hundred cylinders (4 mm x 5 mm) of composite were fabricated using 4 hybrid com-
posites [AeliteFil (Bisco), Prodigy (SDS Kerr), TPH (Dentsply Caulk), and Z100 (3M ESPE)] following manufacturers’
directions and stored for 6 years in 1% NaCl solution. After aging, each specimen was wet polished through 600-grit
SiC and randomly assigned to a self-etching bonding system (Adper Prompt L-Pop/Z100 [3M ESPE]; Tyrian One-Step
Plus/AeliteFil [Bisco]; OptiBond Solo Plus SE/Prodigy [SDS Kerr], Xeno III/TPH [Dentsply Caulk]) or a total-etch
control (Prime&Bond NT/TPH [Dentsply Caulk]) (n = 10 per group). Shear bond strengths (SBS) for repairs were
evaluated after 48 h (crosshead speed = 0.5 mm/min) and were compared by two-way ANOVA (p = 0.05) with Tukey
post-hoc tests.

Results: Significant differences (p ≤ 0.05) were detected for the main effects (substrates and bonding systems),
but the interaction was not significant. SBS for bonding systems were from highest to lowest: (1) Prime&Bond NT,
(2) OptiBond Solo Plus SE, (3) Adper Prompt L-Pop, (4) Xeno III, (5) Tyrian One-Step Plus. SBS of the repair systems
to Z100 were significantly lower than those to the other composite substrates.

Conclusion: Self-etching systems can be used to repair aged composite, but the efficacy of repair of aged com-
posite is system dependent.

Key words: self-etching, composite repair, re-bonding, bond strength.

J Adhes Dent 2005; 7: 159–164. Submitted for publication: 28.05.04; accepted for publication: 16.08.04.

esin-based composites are widely used in restorative

a

b
PhD Candidate, University of North Carolina at Chapel Hill, NC, USA.
Professor, Department of Operative Dentistry, University of North Carolina at
Chapel Hill, Chapel Hill, NC, USA.
c Associate Professor, Department of Operative Dentistry, University of North
Carolina at Chapel Hill, Chapel Hill, NC, USA.
d Assistant Professor, Department of Operative Dentistry, University of North
Carolina at Chapel Hill, Chapel Hill, NC, USA.
e Professor and Chair, Department of Operative Dentistry, University of North
Carolina at Chapel Hill, Chapel Hill, NC, USA.
Reprint requests: Dr. Erica C.N. Teixeira, Department of Operative Dentistry,
School of Dentistry, CB#7450, University of North Carolina at Chapel Hill,
Chapel Hill, NC 27599-7450, USA. Tel: +1-919-966-4604, Fax: +1-919-966-
5660. e-mail: teixeire@dentistry.unc.edu
This study was presented at IADR/AADR in Honolulu March 2004.
R dentistry and continue to evolve with the develop-
ment of more wear-resistant formulations, better adhe-
sives, and improved light-curing and surface-sealing
systems.3 However, fractures and failures of composite
restorations do occur from time to time, and the clinician
must decide whether to replace or simply repair these
restorations.22
Complete removal of defective composite restorations
is not always necessary or desirable. Replacement fre-
quently involves the removal of adjacent tooth structure
in order to optimize the new enamel bond,24 leading to
larger preparations with further loss of tooth structure.18
Repair of an existing restoration is a more conservative
procedure. Repair of fractured and/or worn restorations
and resurfacing of discolored restorations are typically

Vol 7, No 2, 2005 159

Teixeira et al

Table 1 Composition of materials used in this study

Materials Composition

Tyrian One Step-Plus Liquid A: ethanol. Liquid B: 2-acrylamido-2-methyl propane sulfonic acid
Bis (2-(methacryloyloxy)ethyl) phosphate, ethanol
Xeno III Liquid A: HEMA, water, ethanol, silicon dioxide. Liquid B: phosporic acid modified methacrylate resin, UDMA, BHT,
camphorquinone, ethyl-4-dimethylaminobenzoate
Adper Prompt L-pop Liquid 1: Methacrylated phosphoric esters, bis-GMA, camphorquinone, stabilizers. Liquid 2: water, HEMA,
polyalkenoic acid, stabilizers
OptiBond Solo Plus SE Water, ethyl alcohol, alkyl dimethacrylate resins, barium aluminoborosilicate glass, silicon dioxide,
sodium hexafluorosilicate, stabilizers, and activators
Prime&Bond NT UDMA, PENTA, R5-62—1 resin, bisphenol-A dimethacrylate, butylated, silicon dioxide, acetone
AeliteFil Bis-GMA, UDMA; fillers: glass (filler content: 80 wt%)
Prodigy Bis-GMA, TEG-DMA; fillers: barium aluminosilicate (filler content: 79 wt%)
TPH Urethane-modified bis-GMA; fillers: barium silicate (filler content: 77 wt%)
Z100 Bis-GMA, TEG-DMA; fillers: zirconium silicate (filler content: 84.5 wt%)

Technical information from manufacturer’s literature

accomplished by the addition of new composite over MATERIALS AND METHODS

existing material.26
Studies have shown that once a composite surface has
been altered (ie, contaminated, polished, or aged) the
bond strength of new composite is compromised.5,8,9,26
Interfacial repair bond strengths are widely variable and
typically in the range of 25% to 80% of the cohesive
strength of the substrate materials.2,5,8,12,19,20,28 Clini-
cally acceptable values are difficult to determine in vitro,
but comparisons between different repair strengths sug-
gest that certain combinations of materials might lead to
weaker restoration than others, and should be avoided.
Some studies have shown that repair bond strength can
reach similar values to shear bond strength of the com-
posite/enamel interface, being therefore clinically accept-
able.4,7,21
A variety of chemical and mechanical surface treat-
ments and bonding agents have been evaluated to repair
composites. The use of an intermediate bonding agent
has been shown to play an important role to enhance the
repair bond,8,16,20,27,28 especially when the surface of
the substrate material is roughened before it is re-
paired.8,9,26-28
Currently, a variety of self-etching bonding systems is
available in clinical practice. These systems contain acid-
ic monomers to demineralize and infiltrate dental hard tis-
sues simultaneously6,11 and are used to bond composite
to both dentin and enamel.11,13 Conceivably, these sys-
tems could be used to repair worn and/or discolored com-
posite surfaces. However, to date no study has been
done to assess their viability in this application. The pur-
pose of this study was to investigate the effectiveness of
self-etching adhesive systems for composite re-bonding
procedures onto different composite substrates that had
been aged for 6 years prior to testing.
The experimental design included 4 popular hybrid com-
posites from the mid-1990s that were polymerized, pol-
ished, and stored for 6 years to be used as experimental
surfaces for re-bonding procedures. These were repaired
with a combination of different bonding systems, includ-
ing 4 self-etching bonding systems and 1 total-etch con-
trol, coupled to the same composite repair materials as
the original substrates. The “sandwich” of old composite,
bonding system, and new composite was tested for shear
bond strength.
Two hundred composite cylinders were fabricated from
each type of composite (n = 50) (see Table 1) by inserting
each material into a PMMA mold (4 mm depth x 5 mm
diameter). The mold was overfilled by about 1 mm so that
the oxygen-inhibited layer would be removed during me-
chanical polishing. Composite cylinders were visible light
cured (XL 1500, 3M ESPE, St Paul, MN, USA) according
to the manufacturers’ recommendations. This procedure
mimicked an earlier model published by Crumpler et al.9
Aging of composite substrates was achieved by immer-
sion in an aqueous 1% sodium chloride solution (Mallinck-
rodt Baker, Paris, KY, USA) at 23°C for 6 years. pH readings
of the storage solution were performed in the lab, and
ranged from 6.8 to 7.3. After aging, specimens were resur-
faced using SiC abrasives to simulate repair of a restoration
that had been in clinical service for a long period of time.
Experimental surfaces were wet polished through
600-grit SiC abrasive and randomly assigned to one of
five repair systems. The repair systems included 4
self-etching bonding systems with a corresponding com-
posite: Adper Prompt L-Pop and Z100 (3M ESPE); Tyrian
One-Step Plus and AeliteFil (Bisco); OptiBond Solo Plus
SE and Prodigy (SDS Kerr), Xeno III and TPH (Dentsply

160 The Journal of Adhesive Dentistry

 Teixeira et al

Table 2 Manufacturers’ guidelines for adhesive systems used for repairs

Adhesive System Manufacturer Directions for use Batch Number

Tyrian One-Step Plus Bisco, Schaumburg, IL, Two coats of Tyrian SPE applied (10 s) and patted dry with foam pellet. 0200006575
USA Two consecutive coats of the adhesive then applied (10 s), air dried
(10 s), and light cured (10 s).
Xeno III Dentsply Caulk, Adhesive applied (20 s), air dried (2 s) and light cured (10 s). 0302000573
Milford, DE, USA
Adper Prompt L-Pop 3M ESPE One coat of adhesive applied (15 s), lightly air dried (15 s), and light 142067
St Paul, MN, USA cured (10 s).
OptiBond Solo Plus SE SDS Kerr Self-etching primer applied (15 s), air dried (3 s), covered with adhesive 207229
Orange, CA, USA (15 s), air thinned (3 s), re-applied (15 s), air dried (3 s), and light cured
(20 s).
Prime Bond NT Dentsply Caulk, Adhesive applied (20 s), air dried (5 s), and light cured (10 s). 020501
Milford, DE, USA

Technical information from manufacturers’ literature

Caulk). A total-etch adhesive system, Prime & Bond NT,

was used with TPH (Dentsply Caulk) as a control (Table 2).
A Mylar strip with a 4-mm hole was used as a spacer
and template. It was placed on top of experimental com-
posite surfaces to obtain a controlled surface area for
bonding with a uniform adhesive thickness.9 In the con-
trol group, the surfaces were treated with 37% phosphoric
acid for 15 s, rinsed for 15 s, and gently air dried for 5 s
(without desiccation) before application of the adhesive
system. For the other groups, application of the bonding
materials was managed as described in Table 2.
An alignment fixture was used to hold cylinders of old
composite, adhesive, and new composite together during
each step of fabrication and during light curing. Speci-
mens were stored in the same sodium chloride solution
at 23°C until testing after 48 h.
Shear bond strength testing was performed using a
universal testing machine (Model 4411, Instron, Canton,
MA, USA) at a crosshead speed of 0.5 mm/min. Each
specimen was clamped into a fixture for alignment so that
a shear load could be applied parallel to the bonded inter-
face (Fig 1). Re-bond strengths (MPa) were calculated as
the maximum load at failure divided by the geometric
cross-sectional area of the hole in the spacer.
Fractured surfaces were examined visually to classify
the mode of failure (adhesive, cohesive). Adhesive failure
Fig 1 Fixture (vise) for holding the specimen (substrate/spacer/
was defined as debonding at repaired interface. Cohesive new composite) and aligning the test interface parallel to the knife
failure was defined as fracture through the composite edge for shear bond strength testing.
restorative material.
Data were analyzed with two-way ANOVA (p = 0.05) to
test for adhesive and substrate effects and its interac-
tion. Tukey’s post-hoc tests were used to determine differ- differences among bonding systems and among sub-
ences between specific means. strates (p ≤ 0.05), but there was no significant interac-
tion between substrate and bonding materials (p = 0.09).
Individual means in Table 3 show the combined contribu-
RESULTS tions of substrate and bonding system. The data were
pooled by substrate and bonding system, and the pooled
Mean shear bond strengths for each repair system are means are shown at the ends of the rows and columns in
reported in Table 3. Two-way ANOVA revealed significant Table 3.

Vol 7, No 2, 2005 161

Teixeira et al

Table 3 Repair shear bond strength (MPa, mean ± standard deviation) for different adhesives to aged composite substrates (6 years old)

Repair Materials (Adhesive + Composite)

Composite Substrates Tyrian One-Step Xeno III Adper Prompt OptiBond Solo Prime&Bond NT
↓ Plus L-Pop Plus (SE)
AeliteFil TPH Z100 Prodigy TPH Substrate
(pooled)

AeliteFil 18.1 (4.5) 16.4 (3.9) 17.9 (1.8) 18.7 (1.8) 21.9 (3.1) 18.6 (3.5)A
Prodigy 16.4 (5.2) 19.0 (4.6) 16.3 (3.3) 19.4 (3.5) 19.0 (8.4) 18.0 (5.3)A
TPH 16.3 (3.8) 16.3 (6.2) 21.5 (5.1) 21.8 (2.2) 20.8 (4.7) 19.3 (5.1)A
Z100 11.6 (3.1) 15.2 (6.8) 12.5 (3.9) 15.3 (3.0) 19.2 (4.2) 14.7 (5.0)B
Repair Material (Pooled) 15.5 (4.7)c 16.7 (5.5)bc 17.1 (4.8)bc 18.7 (3.5)ab 20.2 (5.3)a

For each test combination, n = 10 specimens. Two-way ANOVA revealed that there was no significant interaction between repair materials and substrate effects. Statistically significant
differences are shown by different superscript letters (p ≤ 0.05). Small superscript letters are used to compare different repair material means. Capital superscript letters are used to
compare different substrate means.

Table 4 Number of cohesive/adhesive failures per experimental group

Repair Materials (Adhesive + Composite)

Composite Substrates Tyrian One Step Plus Xeno III Adper Prompt L-Pop Optibond Solo Plus (SE) Prime Bond NT
↓ Aelitefil TPH Z100 Prodigy TPH

AeliteFil 3/7 1/9 1/9 8/2 4/6

Prodigy 0/10 0/10 0/10 2/8 2/8
TPH 0/10 0/10 1/9 1/9 1/9
Z100 1/9 2/8 2/8 0/10 4/6

C/A-cohesive/adhesive

Pooled values of re-bond strengths according to the
bonding systems were ranked from highest to lowest as
Prime&Bond NT > OptiBond Solo Plus SE > Adper Prompt
L-Pop > Xeno III > Tyrian One-Step Plus. Statistically signif-
icant differences (Tukey’s test, p ≤ 0.05) were found
between the control group and the self-etching groups, with
the exception of OptiBond Solo Plus SE. Tyrian One-Step
Plus and OptiBond Solo Plus SE did not differ from Xeno
III and Adper Prompt L-Pop, but were statistically different
from each other. Tukey’s test showed that the bond
strengths of the repair systems to Z100 were significantly
lower than those to the other substrates (p ≤ 0.05). Exam-
ination of the fractured surfaces revealed that 16.5% were
cohesive failures in the restorative composite, while 83.5%
were adhesive failures at the repaired interface. The exact
number of each failure mode (cohesive and adhesive) per
group is shown on Table 4. The greatest amounts of cohe-
sive failures were observed in the Prime&Bond NT and
OptiBond Solo Plus SE groups (11 each).
DISCUSSION
The present study was based on a shear bond strength
model originally reported by Crumpler et al.9 Specimens
were relatively easy to fabricate using the alignment
fixture during the materials’ handling procedures and
subsequent curing. Measured shear bond strengths for
repaired composite systems were in the typical range (15
to 25 MPa) of resin bonds to enamel and dentin.6,11,13
Some studies reported slightly higher values (25 to
38 MPa)22,27 than the ones observed, which may be
related to the aging time of the composite substrates
employed in our study. Different procedures used to treat
the composite surface before repairing it, such as silana-
tion and sandblasting, can also influence the repair
bond.9,26,27 However, it has been established that rough-
ening of the composite surface plus the use of an inter-
mediate bonging agent should produce acceptable bond
strength.8,9,16,21,22,26
The primary focus of the study was to evaluate the
effectiveness of different adhesive systems and com-
posites for repairing aged composites. Several previous
studies have recommended application of intermediate
materials (ie, bonding systems) to improve bond strength
for repairs.5,7,10,14,17,22,28 The new self-etching bonding
systems are easy to apply11,13 and can be used to condi-
tion both the surrounding tooth and the composite to be
repaired in one procedure, showing an ideal clinical sce-
nario. However, long-established bonding agents based

162 The Journal of Adhesive Dentistry


on chlorophosphate esters of bis-GMA have proven to be
acceptable choices as intermediate materials. The polar
nature of the phosphate groups might contribute to bond-
ing with the inorganic filler component of composites.22
In a repair, there are opportunities for both mechanical
and chemical bonding. Micromechanical interlocking of
new material into the surface roughness features on old
composite is certainly possible, although some studies
demonstrated that abrading the specimens did not make
a significant difference in the repair strength.5,10,19 Part of
the reason for this might be that abrading may generate a
smear layer which is difficult to remove and could interfere
with good bonding. Three chemical mechanisms are pos-
sible as well.9 In each case, an adhesive layer is assumed
to bridge the interface from the old to new composite. The
mechanisms include: (1) formation of chemical bonds be-
tween the new bonding system with the old and new com-
posite matrix; (2) formation of chemical bonds between
the new bonding system and surfaces of exposed filler par-
ticles within both the old and new composite; and (3) mi-
cro-entanglement of new bonding system polymer chains
with the polymer matrix of old and new composite. The last
mechanism most likely dominates and could produce the
greatest contributions to bonding.14,24,25
Once a bonding system polymerizes, newly formed
matrix polymer could become entangled or intertwined
with old composite matrix polymer. Separating the bond-
ed materials would require breaking chemical bonds,
even if no old and new polymer were chemically reacted
to the bonding system. This would generate appreciable
strength.14 The ability of the monomers and solvent
systems to penetrate into the old composite surface
depends on the chemical affinity of the materials and the
degree of hydration of the old composite.9,14 Most com-
posites are hydrophobic in nature but contain some
absorbed water that might improve surface penetration by
hydrophilic bonding systems such as the current class of
self-etching primers.
Self-etching systems do not perform equally well when
bonded to dental structures. For both dentin bonding and
re-bonding for repairs, it is crucial that the intermediate
bonding system wet the substrate surface and employ a
solvent that encourages bonding system monomer to
penetrate into the substrate.15,20 Both of these key
factors are influenced by the application protocol that
might include multiple applications, longer dwell times,
and more careful solvent drying. OptiBond Solo Plus SE
has been reported to display higher bond strengths com-
pared to some other self-etching systems.6 Because this
adhesive is applied twice with a light brushing motion
over 15 s, this may allow easier penetration of the sol-
vent and monomer into the surface being repaired. It is
key that the repair materials wet the substrate to gener-
ate good repair bond strength.15,20 Low-viscosity filled
adhesives have been demonstrated to have a high capac-
ity to wet composite surfaces and penetrate the organic
phase of the composite.15 In the present study, the high-
est SBS values were achieved with Prime&Bond NT and
OptiBond Solo Plus SE, both filled adhesives. However,
Vol 7, No 2, 2005
Teixeira et al
Tyrian One-Step Plus and Xeno III are also filled adhe-
sives, but their SBS values were closer to Adper Prompt
L-Pop, which is an unfilled adhesive.
Not all composite substrates were equal in their ability
to be repaired. Lower SBS values were observed for bond-
ing systems used with Z100. More highly hydrophobic
matrices, more advanced monomer-to-polymer conver-
sion, and more highly filled formulations for composites
may all discourage opportunities for penetration of bond-
ing systems into cured composite substrates. One might
guess that shorter and shorter bonding agent application
times would make penetration even more unlikely. There-
fore, some of the newest self-etching primers and
self-etching bonding systems might not work well for
repairing composites at all. These problems need to be
more carefully considered.
Water sorption also has a complex and deleterious
effect on the integrity and properties of polymer matrix
composites, including flexural and repair strengths.16,25
Presumably, the long period of aging in the present study
makes it a much more realistic simulation for repair of
older composite restorations. To mimic the ionic charac-
ter of saliva, an aqueous NaCl solution was chosen as
the storage medium rather than water.
Although it has been shown that different monomers
or monomers mixtures are responsible for the degree of
conversion in dental composite materials, all the materi-
als used as the repair substrates have similar monomer
composition. Bis-GMA has been demonstrated by FTIR to
have the least degree of conversion, and therefore could
have more unreacted double carbon bonds, favoring a
better repair bond strength.23 However, their apparent
reactivity decreases due to steric hindrance.1 Therefore,
it is difficult to determine how much effect the unreacted
bonds in the composite substrates would have on the
results. The effect of a mechanical interlock between the
matrices and the bonding systems seems to be a more
reasonable assumption than a chemical bonding.
Ideally, the SBS for a repair should be the same as the
bulk shear strength of the composite substrate. Yet,
reported repair strengths are much lower than average
bulk shear strengths.5,10,12 There could be different ex-
planations for this. Newer bonding materials are designed
to be hydrophilic for wetting dentin and may not have op-
timal properties for wetting and absorption into hydropho-
bic composites. Older composite matrices might have
changed during aging and be less able to mechanically or
chemically bond during repair procedures. Finally, at the
site of a repair an interface is produced that is predomi-
nantly the composition of the bonding system compo-
nent, and that may be the weakest link. Cracks during fail-
ure tend to propagate along a path of least resistance.
From the post-test failure analysis, 83.5% of the fracture
surfaces were adhesive involving the interface of the
bonding system. If the bulk SBS for the bonding system
is much lower, then repair strengths in the range of 15 to
25 MPa might be expected. If this interface becomes thin-
ner and thinner, then the repair may mimic the strength of
the composites instead.
163
Teixeira et al
The repair values fell within the range of 15 to 25 MPa,
typical of resin-dentin bonds, and therefore are probably
clinically acceptable in most instances. The actual mech-
anism of interfacial failure during debonding is not well
known, but is hypothesized to involve defects along the
interface that initiate cracks. Defects can arise from
voids, heterogeneities in structure, sites of contamina-
tion, and a myriad of other factors. At the moment, none
of these factors are well characterized.
Finally, to understand the true mechanism of adhesion
during composite repairs and the impact of clinical vari-
ables during repair procedures, it is critical to look more
carefully at the microscopic details of the interaction
between the bonding materials and resin matrix of the old
composite. As noted earlier, penetration of bonding mate-
rials into composite would seem to be the rate-limiting
step. One might expect that a resin interdiffusion zone or
hybrid zone of bonding agent and old composite should
occur at interfaces. However, none of this has yet been
characterized for composites.
CONCLUSION
Repair procedures for aged substrates can be performed
using a self-etching resin bonding system and new com-
posite, but the shear bond strength of the repaired inter-
face is dependent on the adhesive used.
ACKNOWLEDGMENTS
The authors gratefully acknowledge 3M ESPE, Bisco, Dentsply Caulk, and SDS
Kerr for providing materials for this study.
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The Journal of Adhesive Dentistry