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Original Article

A comparative effect of various surface chemical

treatments on the resin composite-composite
repair bond strength
Shaloo Gupta, Abhishek Parolia1, Ashish Jain2, Kundabala M2, Mandakini Mohan1,
Isabel Cristina Celerino de Moraes Porto3
Department of Prosthodontics, Manipal College of Dental Sciences, Manipal, Karnataka, India, 1Division of Restorative Dentistry, School
of Dentistry, International Medical University, Kuala Lumpur, Malaysia, 2Department of Conservative Dentistry and Endodontics,
Manipal College of Dental Sciences, Mangalore, Karnataka, India, 3Department of Restorative Dentistry, Federal University of Alagoas,
Maceio, Alagoas, Brazil

ABSTRACT Address for correspondence:

Dr. Abhishek Parolia,
Aim: The aim of this in vitro study was an attempt
School of Dentistry, International Medical University,
to investigate the effect of different surface Bukit Jalil 57000, Kuala Lumpur, Malaysia.
treatments on the bond strength between pre- E-mail: abhishek_parolia@imu.edu.my
existing composite and repair composite resin.
Materials and Methods: Forty acrylic blocks were
prepared in a cuboidal mould. In each block, Access this article online
a well of 5 mm diameter and 5 mm depth was Quick response code Website:
prepared to retain the composite resin (Filtek™ www.jisppd.com
Z350, 3M/ESPE). Aging of the composite discs DOI:
was achieved by storing them in water at 37°C
10.4103/0970-4388.160402
for 1 week, and after that were divided into 5
PMID:
groups (n = 8) according to surface treatment:
Group I- 37% phosphoric acid, Group II-10% ******

hydrofluoric acid, Group III-30% citric acid,

Group IV-7% maleic acid and Group V- Adhesive
(no etchant). The etched surfaces were rinsed and
dried followed by application of bonding agent
(Adper™ Single Bond 2. 3M/ESPE). The repair
composite was placed on aged composite, light-
cured for 40 seconds and stored in water at 37°C
for 1 week. Shear bond strength between the aged
and the new composite resin was determined with
a universal testing machine (crosshead speed of 0.5
mm/min). Statistical Analysis: The compressive
shear strengths were compared for differences
using ANOVA test followed by Tamhane’s T2 post
hoc analysis. Results: The surface treatment with
10% hydrofluoric acid showed the maximum bond
strength followed by 30% citric acid, 7% maleic
acid and 37% phosphoric acid in decreasing order.
Conclusion: The use of 10% hydrofluoric acid can
be a good alternative for surface treatment in
repair of composite resin restoration as compared
to commonly used 37% orthophosphoric acid.
KEYWORDS: Composite resins, dental restoration
failure, dental restoration repair, operative dentistry
Introduction
Esthetics has become a prime concern among people
in recent past. To fulfill these demands, various types
of tooth color restorative materials have been tried
out. Among these materials, composite resin is the
most commonly used nowadays. Composite resins
have been introduced into the field of conservative
dentistry to minimize the drawbacks of the acrylic
resins that replaced silicate cements (the only esthetic
materials previously available) in the 1940s. It can be
used almost anywhere in the mouth for any kind of
restorative procedure. The reason for such expanded
usage of these materials relates to improvements in
their ability to bond to the tooth structure and their
physical properties. Dental composite resin consists
of a monomeric matrix resin, silanated inorganic
fillers, a polymerization initiator system, inhibitors
for storage stability and pigmentation for shading.[1]
Although marked improvements have been noted in
terms of physical and mechanical properties during
the last 10-20 years, enzymes present in the oral
cavity, for instance, can degrade the composite
matrix.[2,3] Moreover composites are less stable in fluids

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Gupta, et al.: Repair of composite resin restoration
and their degradation rate is higher in saliva simulating
conditions, depending on the chemical nature of the
monomers, amount of dimers and oligomers, the
degree of cross-linking in the polymerized matrix, and
other intraoral impact.[4,5] Also, fatigue can accelerate
the wear process in composite materials. All these
factors result in discoloration, microleakage, wear,
ditching at the margins in clinical situations, which
in turn, may require repair or replacement of the
restoration.[6,7]
Replacement of dental restorations is still common in
daily dental practice due to problems like secondary
caries, fracture of restoration, fracture of tooth,
marginal staining of tooth, marginal defect of the
restoration, partial loss of restoration and patient
request for esthetics.
However, replacing restorations has many
disadvantages such as being time-consuming;
unnecessary removal of the healthy tooth structure
and damage to the pulpal tissues.[8,9]
Repair as an alternative to complete removal is
justifiable because it preserves the tooth structure. It
is often difficult to remove an adhesive restoration
without removing an integral part of the tooth.
However it is not followed widely as the criteria
of repairing restorations are still controversial and
not widely taught in dental schools. According to a
study conducted by Yousef and Khoja[10] 70.7% of the
participants were taught the indications for the repair
of composite restorations only 43% of them actually
repaired restorations. It was also revealed that 30.4%
participants did not repair dental restorations as they
had no clinical experience; 28.3% performed repairs
on their supervisor’s recommendation, 18.5% did not
perform the procedure due to the lack of evidence and
8.7% due to poor clinical experience.
While the clinical procedures for bonding of resin
composites to enamel and dentin as well as to
restorative materials such as metal and ceramic are
well established, there is still no consensus regarding
the most effective protocol for bonding a repair resin
composite to an existing composite restoration. A
strong and durable composite-to-composite bond
is not as difficult to establish as it may appear from
the fact that the chemical composition of the resin
composite serving as the substrate and the bonded
resin composite is basically identical. As a result of the
limited number of reactive methacrylate groups after
polymerization and water sorption into the preexisting
composite, the repair composite cannot effectively
bond to aged restorations without adequate surface
treatment.[11] A number of surface treatment protocols
have been proposed to improve repair bond strength
in between aged and nonaged composite resins,
which include grinding, acid etching and sandblasting
followed by different types of adhesive treatments,
246 Journal of Indian Society of Pedodontics and Preventive Dentistry | Jul-Sep 2015 | Vol 33| Issue 3 |
with conflicting results.[1,12-15] Hence, the aim of this in
vitro study was an to investigate the effect of different
surface treatments on the bond strength between
preexisting composite and repair composite resin.
Materials and Methods
A block of Filtek™ Z350 composite resin (3M/ESPE,
Minnesota, United States of America) was bonded to a
newly block of Filtek™ Z350 composite resin (3M/ESPE,
Minnesota, United States of America) by application of
five different etchants as a surface treatment followed
by Adper™ Single Bond 2 adhesive agent (3M/ESPE,
Minnesota, United States of America). Each specimen
was light-irradiated using a halogen curing light
(Spectrum 800, Dentsply DeTrey, Konstanz, Germany)
with light output of 500 mW/cm2 as measured with a
curing radiometer (Demetron/Kerr, Danbury, United
States of America) was used to cure all specimens.
Preparation of the specimen
A total of 40 acrylic blocks were prepared in stainless
steel cuboidal mold of dimension 50 mm in length,
15 mm width, and 10 mm height. The exposed test
surfaces of the repair groups were wet-polished with
220, 320 and 400 Carbide polishing paper (Metatech
Industrial Consumbles, Maharashtra, India). In each
block, a well of 5 mm diameter and 5 mm depth was
prepared to retain the composite resin. Each well was
filled with composite resin in increments of 1.0 mm
thickness and cured for 40 s. Aging of the composite was
achieved by storing them in water at 37°C for 1 week.
After this 40 wells were divided into five groups (n = 8)
and surface treatment was done, as follows:
Group I:  Etched with 37% phosphoric acid, Total
Etch (Ivoclar Vivadent Inc., Schaan,
Liechtenstein) for 60 s.
Group II: Etched with 10% hydrofluoric acid,
Porcelain Etch Gel (Pulpdent Corp.,
Massachusetts, United States of America)
for 60 s.
Group III: Etched with 30% citric acid for 60 s (the
citric acid formulation was prepared by
Manipal Pharmacy, Mangalore, Karnataka,
India).
Group IV: Etched with 7% maleic acid for 60 s (the
maleic acid formulation was prepared by
Manipal Pharmacy, Mangalore, Karnataka,
India).
Group V: Control, no etching.
The etched surfaces of preexisting composite resin
were rinsed with a jet of water and dried using an air
spray. This was followed by application of a layer of
Adper™ Single Bond 2 adhesive system (3M/ESPE,
Minnesota, United States of America). The surfaces
were then light-cured for 20 s with the same light
curing the source. The repair of Filtek™ Z350 composite
resin (3M/ESPE, Minnesota, United States of America)
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Gupta, et al.: Repair of composite resin restoration

was placed on aged composite using split mold (5 mm Table 1: Variation between shear strengths of
diameter) and light-cured for 40 s. The blocks were the five groups using ANOVA
again stored in water at 37°C for 1 week to simulate
n
Mean SD SE F P value
the oral environment and shear bond strength (MPa)
measurements were made. Control 8 8.7913 4.77780 1.68921 5.111 0.003
Citric acid 8 14.2900 3.79950 1.34333
Shear bond strength test Hydrofloric acid 8 16.9400 5.01452 1.77290
Shear bond strength test was done by a universal Maleic acid 8 10.6313 2.75896 0.97544
testing machine, Instron Model 4411 (Instron Corp., Phosphoric acid 8 10.57 4.07 1.66
Massachusetts, United States of America) with a Total 40 12.1268 4.80822 0.76025
crosshead speed of 0.5 mm/min. A stainless steel blade SD = Standard deviation; SE = Standard error; ANOVA = Analysis of
1 mm thickness with 45° inclination at the tip was variance
adapted at the interface of the aged and new composite
cylinders. The direction of the force was perpendicular
to the long axis of specimens. The shear bond strength Table 2: Tamahne’s T2 post hoc analysis
value was calculated in Megapascal (Mpa). Comparison A Comparison Mean SE Significant
with difference
Control Citric acid −4.30875 1.61495 0.185
Statistical analysis Hydrofloric acid −6.95875 1.98663 0.05
The normality of the distribution was assessed by
Maleic acid −0.65000 1.32477 1.000
Shapiro–Wilk’s W-test. Compressive shear bond
Phosphoric acid −0.59542 1.88980 1.000
strengths values were analyzed using analysis of
Citric acid Hydrofloric acid −2.65000 2.22434 0.947
variance F-test, followed by Tamhane’s T2 test for
Maleic acid 3.65875 1.66012 0.379
pairwise comparisons between the means, at a
Phosphoric acid 3.71333 2.13830 0.694
significance level of 0.05. Statistical Package for the
Social Sciences (SPSS) software, version 17.0 (SPSS, Hydrofloric Maleic acid 6.30875 2.02353 0.095
acid Phosphoric acid 6.36333 2.43125 0.205
Chicago, IL, United States of America) was used for all
SE = Standard error
statistical analyzes.

Results remaining healthy tooth structure, is a more suitable

The shear bond strengths of control and all the acids used
except maleic acid group showed normal distribution.
All five groups showed significant variation between
shear bond strengths with F = 5.111 and (P = 0.003)
as indicated in Table 1. The results of the shear bond
strengths for different surface treatments and control
groups are shown in Table 2. Among the five groups
used, hydrofluoric acid showed the maximum bond
strength with a mean of 16.94 Mpa, followed by citric
acid 14.29 Mpa, maleic acid 10.63 Mpa and phosphoric
acid 10.57 Mpa in decreasing order. The’s T2 post
hoc analysis showed that the significant difference
was observed in between hydrofluoric acid and the
control group (P < 0.05) indicating its superiority to
other etchants used. The specimens treated with citric
acid, maleic acid, and phosphoric acid did not show
any significant difference from the control group
(P > 0.05). There were no significant differences among
all specimens treated with different acids [Table 2].
Discussion
Establishing a strong and durable composite-to-
composite bond is not as trivial as it may appear from
the aspect that the chemical composition of the resin
composite serving as the substrate and the bonded
resin composite is basically identical.[12] Thus repairing
the composite restoration rather than replacing the
whole restoration, which involves destroying the
treatment option. It is considered minimal invasive
and cost effective treatment, which not only prolongs
the service life of aged composite restorations, but also
is more acceptable to the patients.[1]
In the present study, composite resin was repaired
with the same type of composite resin using different
etchants. It is known that in repair of composite resin
restoration, the new composite resin cannot effectively
bond to the aged, polished composite resin because of
the limited number of reactive methacrylate groups left
in the preexisting composite resin after polymerization
and water sorption. Therefore, to achieve the better
outcome it is essential to roughen this polished surface
of preexisting composite resin by using adequate
surface treatment.[11]
As the bond strength of composite to the etched enamel
has been reported to be about 15–30 Mpa, hence the
repair bond strength of composite resin restoration
should not be less than this value.[16] According to Brosh
et al.[17] the bonding of old and new composite resin,
occur by three distinct means, that is, chemical bonding
with the organic matrix, chemical bonding with
exposed filler particles and through micromechanical
retention to the treated surface. As it is known that
a strong chemical bond to resin matrix of an aged
composite is questionable and in order to improve
repair bond strength, different surface treatments have
to be used such as silica coating, phosphoric acid etching
followed by an adhesive, hydrofluoric acid etching,

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Gupta, et al.: Repair of composite resin restoration
abrasion, and sandblasting.[17] Sandblasting and
etching with hydrofluoric acid are reliable methods to
bond composite to porcelain.[18,19] However, studies on
the repair strength of composite resins using different
etching agents are very few. This study compared
different etchants such as 10% hydrofluoric acid, 30%
citric acid, 7% maleic acid and 37% phosphoric acid
and it was revealed that hydrofluoric acid provided
the best repair bond strength among these etchants.
Hydrofluoric acid being a strong acid etches amorphous
SiO2, quartz or glasses and commonly used to etch
ceramic dental restorations to improve bonding in their
repair.[20] It reacts with and remove, the glassy matrix
that contains silica. This leaves the crystalline phase
exposed and thus increases the surface roughness.
This process also results in enhanced wettability and
surface energy on the ceramic surface allowing greater
penetration of the resin cement tags. This results in
increased bond strength between the ceramic and
cement. The same applies to composite, which has
silica as filler. Commonly used 37% phosphoric acid
is not as efficient in removing silica as hydrofluoric
acid.[21] Thus, it was justifiable to use hydrofluoric
acid for repair of composite resin. It results in a better
bond strength if used at the desired concentration
that is 4-10% hydrofluoric acid. The results of the
present study is in disagreement with the study done
by Lucena-Martín et al.,[22] in which the application of
hydrofluoric acid as a surface treatment in the repair of
composite resin has shown lower shear bond strength.
This could be due to the duration of the application of
hydrofluoric acid on the surface. In the present study
hydrofluoric acid was used for 1 min on the substrate
and that seems to favor the high bond strength with the
new composite resin while Lucena-Martín et al. applied
hydrofluoric acid for 2 min. However, hydrofluoric
acid is contraindicated on dentin because it blocks the
dentinal tubules by forming star-like structures, which
in turn degrades the bond strength of composite resin
to the tooth structure.[23,24]
Potential hazards of hydrofluoric acid known from
other applications than dentistry should be considered
also in dental applications. Hydrofluoric acid can be
harmful due to its ability to readily penetrate skin tissues
(often without causing an external burn). The damage
is directly related to the concentration of the acid and
the duration of contact. Erythema and pain may be
delayed up to 24 h in exposure to dilute hydrofluoric
acid solutions (<20%). In high concentration (>21%) it
can cause extensive internal tissue damage, as well as
alter blood calcium levels (due to the formation of CaF2),
which can lead to dangerous heart arrhythmias.[25] But,
a concentration range of 4-10% can be used safely for
dental procedures such as intraoral repair, provided
caution is taken to use appropriate barrier techniques,
viscous hydrofluoric acid gel formulations, and
continual visual observation during the application
period.[21,25] Other etchants such as 30% citric acid, 7%
maleic acid and 37% phosphoric acid have also been
used in the past with varied results.[1,12,14,20] The results
248 Journal of Indian Society of Pedodontics and Preventive Dentistry | Jul-Sep 2015 | Vol 33| Issue 3 |
of this study showed that the synergic effect between
chemical surface treatment with the most commonly
used etchant that is, 37% phosphoric acid and dentin
bond agent exhibited significantly less bond strength
as compared to etchants like 7% maleic acid and 30%
citric acid. This finding agrees with previous study
that phosphoric acid group reached the lower MPa
values.[20] It could be possibly due to the insufficient
amount of residual monomers left in aged composite,
required to promote a strong chemical bond by
participating in the chemical reaction with the new
composite resin, thus a greater surface roughness is
required to increase micromechanical retention that
phosphoric acid was not able to provide.[1]
Conclusion
To repair a composite resin restoration, 10% hydrofluoric
acid can be a good alternative for surface treatment as
compared to commonly used 37% orthophosphoric
acid. However, proper protocol entails the application of
an adhesive agent following the acid etching procedure
as the latter alone cannot produce an effective bond of
aged composite to repair composite.
Acknowledgment
This study was supported by 3M ESPE, India.
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How to cite this article: Gupta S, Parolia A, Jain A,
Kundabala M, Mohan M, de Moraes Porto IC. A comparative
effect of various surface chemical treatments on the resin
composite-composite repair bond strength. J Indian Soc Pedod
Prev Dent 2015;33:245-9.
Source of Support: Nil, Conflicts of Interest: None declared.
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