Lasers Med Sci (2013) 28:879–889
DOI 10.1007/s10103-012-1169-1
ORIGINAL ARTICLE
Shear strength of composite bonded to Er:YAG laser-prepared
enamel: an in vitro comparative study
Frank Y. W. Yung & Norbert Gutknecht &
Rene Franzen & Horst Fischer
Received: 22 October 2011 / Accepted: 16 July 2012 / Published online: 2 August 2012
# Springer-Verlag London Ltd 2012
Abstract The primary objective of this study is to investi-
gate the adhesion properties between four current genera-
tions of bonding systems and enamel surface conditioned by
Er:YAG laser, using an energy density comparable to the
ablation threshold of enamel. By including an energy den-
sity comparable to published adhesion studies, the second-
ary objective is to compare the adhesion effects of these
selected laser conditioning parameters on enamel with other
similar published studies. Material and methods: Buccal
sides of randomly selected human molars (N0117) were
prepared and divided into nine experimental groups depend-
ing on the generations of bonding system represented by the
corresponding number (G4, G5, G6, G7) and the additional
laser conditioning on the enamel surface represented by
laser etch (LE) and laser etch with a higher pulse energy,
followed by acid etch (AE), if required. The bonding resin
systems and their specific requirements were applied after
the enamel surfaces were laser conditioned following a
specific set of laser parameters. Composite posts of
1.6 mm in diameter and approximately 6 mm in length were
then restored on each of the sample surfaces. After 48 h, the
F. Y. W. Yung
Aachen University,
Aachen, Germany
N. Gutknecht : R. Franzen
Department of Conservative Dentistry, Periodontology and
Preventive Dentistry, University of Aachen,
Aachen, Germany
H. Fischer
Department of Dental Materials and Biomaterials Research,
University of Aachen,
Aachen, Germany
F. Y. W. Yung (*)
1100 Sheppard Ave. E. Suite 307,
Toronto, ON, Canada M2K 2W1
e-mail: frankyung@rogers.com
composite assemblies were tested to failure under compres-
sion using a knife edge loading head at a cross head speed of
1 mm/min until the composite cylinders were separated
from the surface. The data collected were then analyzed
using one-way analysis of variance and SAS software pro-
gram (9.1, TS1M3). Results: No significant difference was
found among these groups: AE+G4/LEAE+G4, G6/LE+
G6, and G7/LE+G7. Significant differences were found in
the remaining groups: AE+G5/LEAE+G5, AE+G5/LEAE-
H+G5, and LEAE+G5/LEAE-H+G5. The bond strength
results were compared among similar published data and
possible influences from different laser parameters, bonding
systems, and their combined impact on the enamel surface
and its adhesion properties were analyzed. Conclusion: Un-
der our specific settings, additional laser conditioning after
phosphoric acid etch is beneficial to one generation of
bonding resin (G5). There is no significant change or detri-
mental effect to the other three groups (G4, G6, and G7) of
bonding resins with respect to their final bond strength. The
published reports of lower bond strength after additional
laser conditioning may be related to thermal damage or
unfavorable alteration to the enamel surface by excessive
laser energy and the chemistry of bonding systems studied.
These factors will affect the overall wettability and the
subsequent adhesion properties of the enamel surface.
Keywords Adhesion . Surface tension . Er:YAG Laser .
Laser parameters . Thermal damage . Shear bond strength
Introduction
Adhesion is a process by which two substances of different
physical properties are attached to each other and can in-
volve, in many situations, complex physical and chemical
interfacial alterations and interactions [1, 2]. In restorative
880
dentistry, where clinical success depends heavily on the
ability of the resin adhesive to remain bonded to the tooth
substrate, enamel surface conditioning or etching is
designed for adhesion enhancement in many restorative
and orthodontic procedures. The etching process can reduce
the contact angle and the surface tension of the enamel
surface, allowing a low-viscosity intermediate primer or
resin to “wet” or penetrate into the microporosities created
by acid etching [1]. Further improvement of this adhesion
strength may reduce the marginal leakage and its related
consequences of postoperative sensitivity, marginal failure,
and recurrent caries. Tooth structures can then be repaired
closer to the tooth's original strength through mutual adhe-
sion and reinforcement [3]. The practice of adhesion den-
tistry was started in 1955 by Dr. Michael G. Buonocore with
a 30-s exposure of 80 % industrial strength phosphoric acid
on enamel [4]. His idea of “rendering the enamel surface
more receptive” to unfilled resin has sparked significant
advancement in bonding chemistry and made possible the
many generations of bonding resins, such as the etch-and-
rinse and self-etch systems that are available today.
Concurrent with the advancement in adhesion chemistry,
alternative methods to generate more enamel surface area or
microporosity for better resin adhesion have been suggested
including air polishing [5], crystal growth [6], and micro-
etching with pressurized pumice [7]. The physical alteration
of the dental surface was further advanced by the introduc-
tion of Er:YAG laser (wavelength, 2,940 nm) for dental hard
tissue applications in 1989 [8]. The optical energy at this
wavelength is strongly absorbed by water. Based on the
12 % by volume water component in enamel, this tissue
water is rapidly superheated by the incredible laser-to-water
absorption. The optical to thermal energy exchange will
create a rapid phase conversion of water to steam, and the
subsequent buildup of internal pressure from the sudden and
sizable volume expansion—water expands roughly 1,600
times when turning from a liquid state to a gaseous state—
causes the explosive destruction of the inorganic structure
once its tensile strength is surpassed [7–9]. These specific
absorption and rapid expansion properties of water provide
the foundation of the water-mediated photothermal–me-
chanical ablation on the enamel surface by the Er:YAG
laser. The efficient photothermal energy transfer ensures
minimal heat diffusion outside of the irradiated volume
and reduces the possibility of thermal side effects on pulpal
tissues. Along with proper water irrigation and rehydration,
the temperature rise locally is clinically insignificant, and
dental hard tissue preparations can be safely performed
without carbonization [10]. Because of these specific and
desirable laser-to-tissue interactions, the Er:YAG laser was
cleared by the FDA in 1997 for cavity preparation and caries
removal [11]. It was perceived as a possible breakthrough,
but the initial enthusiastic expectations were met with the
Lasers Med Sci (2013) 28:879–889
inconclusive research and clinical results that followed. On
one hand, using the laser was considered a suitable, alternate
technique to etch enamel for restorative and orthodontic
bonding [12–15]. A number of studies have demonstrated
that the Er:YAG laser can etch enamel precisely, with min-
imal thermal damage [16–20]. On the other hand, several
studies have indicated that laser-etched enamel surface
bonded less effectively than conventional phosphoric acid
etching. They have demonstrated that the Er:YAG laser-
etched enamel surfaces produced lower or undesirable bond
strength values as compared to the traditional acid etching
procedures [21–25].
In current dental practices, there are four popular groups
of adhesive systems for composite restorations: etch-and-
rinse fourth and fifth generations and the no-rinse, self-etch
sixth and seventh generations of bonding systems. By add-
ing Er:YAG laser conditioning with a selected set of laser
parameters to their usual application protocol, the primary
objective of this study is to evaluate whether additional laser
conditioning with an energy density close to the ablation
threshold of enamel will enhance the final adhesion of these
four bonding systems. Using another energy density com-
parable to published adhesion studies, the secondary objec-
tive is to compare this group of experimental results among
other published data and explore the possible influences
from different laser parameters and their impact on wetta-
bility and adhesion of the enamel surface. Shear bond
strength was selected among several parameters that could
be used for the evaluation of these adhesions [26]. It is the
measurement of the load-bearing capacity of the restorative–
dental interface and the ability of the adhesion to resist
separation. Comparison of the data can be a good reflection
of how the adhesive resin is interacting with the conditioned
dental surfaces. The final bond strength may be improved if
the surface tension of the enamel substrate is lowered, and
the wettability of the enamel surface is made more favor-
able, allowing the bonding resin to flow and penetrate better
into the etched or conditioned microporosities [27].
Material and methods
Sample preparation
Human third molars without decay, cracks, gross irregular-
ities, or hypocalcified enamel structures that were extracted
within 1 to 2 months prior were selected and preserved in
chloramine-T solution (0.5 %). These samples were washed
in distilled water; soft tissue remnants and calculus were
removed with ultrasonic scalers and cleaned with fluoride-
free pumice in dental prophylactic cups. The roots were
sectioned approximately 2 mm below the cementoenamel
junction, and the hollow pulpal chambers were filled with
Lasers Med Sci (2013) 28:879–889
cotton. Notches were cut at the lingual cervical margin for
surface reference and better acrylic anchorage. They were
then stored in physiological saline solution at 4 °C. A total
of 117 samples were randomly selected from this pool of
prepared teeth, and the buccal surfaces were ground on wet
180-grit silicon carbide papers (Buehler Ltd, Lake Bluff, IL,
USA) to obtain a flat surface. Each sample was mounted in a
polyethylene mold, with the flattened surface parallel to the
base and embedded in a self-polymerizing acrylic resin
(Crosslinked Flash Acrylic by Yates-Motloid Co., USA).
They were placed in water to modify the rise in temperature
during the exothermic polymerization of the acrylic resin.
Each of the enamel surfaces was then polished with 220-,
320-, 400-, and 600-grit silicon carbide papers (Buehler Ltd,
Lake Bluff, IL, USA) under a copious supply of water until
a sufficient enamel surface was obtained. The polished
enamel surfaces were evaluated under a laboratory magni-
fication lens, making sure that there was no dentin exposed.
These procedures were conducted to obtain flat, even, and
standardized smear layers on the enamel surfaces for bond-
ing comparison. Appropriate test sites on the polished enam-
el surface were identified with a circular mark of 3 mm in
diameter with an indelible felt-tip pen. They were then
randomly selected and divided into nine groups, each con-
taining 13 tooth samples and stored in physiologic saline at
37 °C for 24 h before the surface conditioning and bonding
of the assembly.
Enamel surface preparation
1. Laser etch (LE) with Er:YAG laser: The Er:YAG laser
used in this investigation is a solid-state dental laser
(VersaWave by Hoya ConBio, Fremont, CA, USA).
The active medium—erbium-doped yttrium–alumi-
num–garnet crystal rod—is excited by a flash lamp that
can generate free running laser pulses. The laser pulse
duration is fixed at approximately 250–300 μs with a
frequency range of 3 to 50 Hz and a pulse energy range
of 30 to 425 mJ. Since there is a small but persistent
optical energy loss by the absorption of the proprietary
zirconium–aluminum–fluoride delivery fiber and the
quartz contact tip, the true exit power was measured
and monitored by an independent external power meter
(PowerMax 600 by Molectron, Portland, OR, USA).
The quartz contact tip was used in near contact mode
during the surface conditioning with both internal and
external water supplies for optimal substrate rehydration
and as a coolant. The hydration rates of 30 mL/min from
the contact tip and 60 mL/min from the external air–
water syringe, the listed power of 2.1 W (30 Hz and
70 mJ), the true exit power at the quartz contact tip of
1.2 W (30 Hz and 40 mJ), the near contact distance, and
the contact tip diameter of 600 μm were all determined
881
previously from an earlier pilot study which is similar to
another published study [28]; they were all kept consis-
tent throughout the laser conditioning. Using the circu-
lar mark as a reference, the contact tip was kept
perpendicular to the enamel surface for a uniform grid
pattern of lasing for 10 s by a single operator. To ensure
the beam quality, the quartz tips were cleaned, polished,
and examined after each conditioning and the exit pow-
er monitored before any fresh lasing. Power density of
424 W/cm2 or energy density of 14.1 J/cm2 based on the
600-μm contact tip and measured power output was
applied. For the higher pulse energy setting group
(LE-H), the listed power was 5 W (20 Hz and
250 mJ), and the true exit power was 3.4 W (20 Hz,
170 mJ). The corresponding power and energy densities
were 1,202 W/cm2 and 60 J/cm2, respectively. The con-
ditioned surfaces were rinsed thoroughly with filtered
water for 60 s and prepared for either further acid etching
or surface bonding depending on the application protocol.
2. Acid etch with phosphoric acid (38 %): 38 % thixotropic
phosphoric acid gel (Etch-Rite by Pulpdent, MA, USA)
was applied evenly on the enamel surfaces for 15 s. The
conditioned surfaces were rinsed thoroughly with fil-
tered water for 60 s and prepared for surface bonding.
Surface bonding procedures and composite assembly
After the surface conditioning, water was completely re-
moved from the enamel surface by means of oil-free and
filtered compressed air. An opening of approximately
1.7 mm in diameter was isolated, and two to three consec-
utive coats of the bonding resin were immediately applied
with gentle agitation to the conditioned surface lasting 15 to
20 s, depending on the bonding requirements. Each of the
recommended application instructions for the four bonding
adhesives was followed closely. The surface was then gently
air-dried to allow the solvents to evaporate and then light
cured for 10 s. A curing unit (Optilux 400 by Demetron/
Kerr, Danbry, CT, USA) with an output intensity of
600 mW/cm2, which could be monitored periodically with
its built-in power meter, was used for all the light curing
procedures. The combinations of four generations of bond-
ing systems designated by their corresponding number of
generation (G4, G5, G6, and G7) and the enamel surface
conditioning methods used in the study are summarized in
Table 1.
A transparent plastic tube of 1.6 mm inner diameter was
filled with 6–8 mm of microfill composite (Point 4 by Kerr
Corporation, CA, USA) and placed over the treated enamel
surface. The assembly was then subjected to the curing light
for 60 s (20 s from three different directions). After the
samples were stored in physiological saline solution for
882
Table 1 Experimental groups by bonding resins and enamel surface preparations
Bonding resin groups Enamel surface preparations
Regular bonding protocol
New Bond and Photo Bond (G4) AE+G4
Prime & Bond NT (G5) AE+G5
Futurabond DC (G6) G6
Futurabond NR (G7) G7
AE acid etch, LE laser etch, LEAE laser etch and acid etch, LEAE-H laser etch with higher pulse energy and acid etch, G4 to G7 recognized
generations of bonding resin
48 h at 37 °C, the softened plastic tube was then carefully
removed, and a cylinder of composite resin (1.6 mm in
diameter and 6–8 mm high) was constructed on each tooth
sample.
Shear bond strength test
To evaluate the shear bond strength (SBS), the samples were
tested using a standardized testing device (Zwick Universal
testing machine model Z2.5 by Zwick Corp., Ulm, Germany).
The composite assemblies were loaded to failure under com-
pression using a knife edge loading head at a cross head speed
of 1 mm/min until the composite cylinder was separated from
the tooth. These tests were performed by an independent
researcher without prior knowledge of the treatment condi-
tions of the tested samples. The maximum load to failure in
newtons (N) was recorded for each sample, and the SBS was
converted in megapascals (MPa). The external diameters of
the recovered composite cylinders were measured from two
directions with a digital caliper (Absolute Digimatic by Mitu-
toyo, model CD-15DC, England), and the mean radius was
used for the SBS calculations.
Histological appraisal of failure mode
The failed interfaces were evaluated using a stereomicro-
scope (Leica MZ6 from Leica Microsystems GmbH,
Wetzlar, Germany) under a ×40 objective and with support-
ing software (Diskus MZ 6 software from Technisches
Büro, Königswinter, Germany). Visual evidence of the fail-
ure mode was captured by a video camera (HV-C 20A,
Hitachi, Japan) connected to the stereomicroscope, and the
fractured surfaces were grouped by type and site [29].
Failure patterns were classified according to four distinctive
types: type 1, complete adhesive failure at the interface
between the bonding resin and enamel; type 2, partial adhe-
sive failure at the interface and partial cohesive failure
within the bonding structure itself; type 3, complete cohe-
sive failure within the composite structure; and type 4,
partial cohesive failure within the enamel substrate.
Lasers Med Sci (2013) 28:879–889
Addition of laser etch (LE) Addition of laser etch
(higher pulse energy) (LE+H)
LEAE+G4
LEAE+G5 LEAE-H+G5
LE+G6
LE+G7
Statistical analysis
The collected shear bond strength means and standard devi-
ations are listed in Table 2. The mean, standard deviation,
and minimum and maximum values were calculated and
represented by box plots in Fig. 1. Furthermore, a one-
factor analysis of variance model was fitted into the data
to describe the group differences. The between-group factor
has nine levels corresponding to the levels in Table 1. Linear
contrasts were used for analysis, and effects were considered
as significant if the p value did not exceed the 5 % level. We
used PROC MIXED from SAS software program (9.1,
TS1M3) under WINDOWS XP for computing the bond
strength data and Fisher exact test for the failure mode
distribution.
Results
The collected shear bond strength test results and their
standard deviation are summarized per experimental group
in Table 2. They are also represented in box plots in Fig. 1.
The fit statistic shows that the ANOVA model could be
fitted to the data (−2 Res Log 920.2). Furthermore, the
ANOVA model shows overall significant group differences
(nDf 10, dDF 124, F010.63, p<0.0001). This test ensures
that there are overall differences between the experimental
groups and the validity of further statistical analyses.
For bonding resin groups G4 and G5 where acid etching
is part of the application protocol, the differences between
groups acid etch (AE)+G4 and LEAE+G4 were not statis-
tically significant (Table 3) indicating that the addition of
laser etch did not improve the adhesion of this group of
resins. In contrast, the additional laser conditioning in
LEAE+G5 provided significantly higher bond strength as
compared to group AE+G5 with acid etch alone (Table 3).
When the results of group LEAE+G5 are compared to the
group of higher pulse energy (LEAE-H+G5), it can be seen
that the higher pulse energy setting lowered the bond
strength for group G5.
Lasers Med Sci (2013) 28:879–889 883

Table 2 Mean shear bond strength (in megapascals) and standard deviation for the experimental groups

Bonding resin groups Enamel surface preparations

Regular bonding protocol Addition of laser etch (LE) Addition of laser etch
(higher pulse energy) (LE+H)

New Bond and Photo Bond (G4) 22.29±5.34 25.49±7.43

Prime & Bond NT (G5) 32.22±12.50 40.35±16.36 20.08±6.68
Futurabond DC (G6) 11.98±3.55 14.70±2.87
Futurabond NR (G7) 18.52±10.33 19.39±10.98

Values in megapascals show the means±standard deviation

AE acid etch, LE laser etch, LEAE laser etch and acid etch, LEAE-H laser etch with higher pulse energy and acid etch, G4 to G7 recognized
generations of bonding resin

For groups G6 and G7 where acid etching is not part of Discussion

the regular application protocol, the mean bond strengths
after adding laser etch were higher, but the differences
between the non-irradiated groups were not statistically
significant. There was no statistically significant gain from
the use of laser conditioning for both bonding systems
(Table 3).
Patterns of the failure modes of groups G5 and G7
are included in Table 4. Most of the failure patterns
belong to the type 2-mixed adhesive–cohesive failure,
and they are represented quite evenly between the five
groups. Partial cohesive failures within the enamel sub-
strate were found with the additional laser-etched groups
(LEAE + G5, LEAE-H + G5). Overheating the enamel
surface can cause subsurface damage; the weakened
crystal lattice structure caused by this excessive thermal
damage can separate, leading to surface fracture as
demonstrated by higher incidences of type 4 cohesive
fractures within the enamel substrate seen with the
laser-treated groups when compared to conventional
etching groups. The distribution of the failure modes
between the five groups differed significantly (Fisher
exact test, p00.0390).
As demonstrated by Buonocore [3], it is possible to attain
better adhesion for an adhesive by improving the adherent
surface. A porous enamel surface with lower surface tension
can facilitate the infiltration of the unfilled bonding resin.
The strength of this bond depends on the viscosity of the
methacrylate monomer to flow, wet, and penetrate into the
conditioned enamel surface [27, 30]. In our study, four
generations of bonding resin systems with different viscos-
ities and chemical compositions were investigated, and their
ability to wet and penetrate enamel surfaces conditioned by
phosphoric acid, Er:YAG laser, or both was examined. The
shear strength from the micromechanical interlock of resin
to enamel was studied because it represents the functional
stresses being transmitted across the bonded restorative–
dental interface, and this strength was found to be directly
related to the ability of the resin to wet and penetrate the
conditioned enamel surface [31].
The ejection of inorganic particles and the formation of
an irregular surface initiated by Er:YAG laser conditioning
should ideally increase the surface area for subsequent acid
conditioning and resin penetration, yet several studies have

Fig. 1 Box plot of bond

strength (in megapascals) to
enamel by experimental groups.
LE laser etch, AE acid etch,
LEAE-H laser etch with higher
pulse energy and acid etch, G4
to G7 recognized generations of
bonding resin

G4 LEAE+G4 G5 LEAE+G5 LEAE-H+G5 G6 LE+G6 G7 LE+G7

Experimental group
884 Lasers Med Sci (2013) 28:879–889

Table 3 Statistical comparison for nine experimental groups

Experimental group Estimate Standard error DF t value Pr>|t| Statistical analysis

AE+G4 vs LEAE+G4 −3.2019 3.6949 134 −0.87 0.3879 AEG40LEAE+G4, no significant difference
AE+G5 vs LEAE+G5 −8.1258 3.6263 134 −2.24 0.0268 AEG5<LEAE+G5, statistically significant
AE+G5 vs LEAE-H+G5 20.2729 3.3874 134 5.98 <.0001 AEG5>LEAE-H+G5, statistically significant
LEAE+G5 vs LEAE-H+G5 20.2729 3.3874 134 5.98 <.0001 LEAE+G5>LEAE-H+G5, statistically significant
G6 vs LE+G6 −2.7218 3.5435 134 −0.77 0.4439 G60LE+G6, no significant difference
G7 vs LE+G7 −0.8716 3.5435 134 −0.25 0.8061 G70LE+G7, no significant difference

AE acid etch, LE laser etch, LEAE laser etch and acid etch, LEAE-H laser etch with higher pulse energy and acid etch, G4 to G7 recognized
generations of bonding resin

shown that the resin–enamel bond strength of Er:YAG laser-
treated surfaces is highly variable, with some results typi-
cally lower than that attained by conventional acid etching
[21–25]. Based on our results using an energy density
comparable to the ablation threshold of enamel, adding laser
conditioning before acid etching did not significantly im-
prove or lower the adhesion of the fourth-generation (LEAE
+G4) bonding resin (Table 3). The additional laser condi-
tioning did, however, improved the adhesion of the fifth-
generation (LEAE+G5) bonding resin which resulted in
better bond strength as compared to the acid-etch-alone
protocol (AE+G5) (Table 3). Under identical laser and acid
conditioning, the differences in their bond strength results
can only be explained by the viscosity and the chemical
composition of these two resin systems, which can affect the
individual affinity or wettability for the same conditioned
enamel surface. When the same set of results are compared
with similar published results in Table 5, the use of a
relatively low pulse energy of 40 mJ and energy density of
14 J/cm2 in our study has shown to be sufficient and,
perhaps, more effective in terms of bond strength enhance-
ment. Some of the published reports have suggested the
possibility of by-product blockage as a cause for their dis-
appointing results, and that mechanical removal of these
loosely attached particles was required in exchange for
higher bond strengths [32, 33]. The sources of these
reported blockages of loosely attached, fused crystalline
enamel particles and asperities by laser conditioning may
be excessive laser energy and an inadequate water rehydra-
tion rate. Compared to a uniform chemical exposure of a
layer of phosphoric acid liquid on enamel, the physical
surface exposure and interaction to the incident laser beam
can be relatively very uneven, even with a nearly ideal laser
beam profile (Gaussian transverse electromagnetic mode
TEM00). The usual clinical beam profiles are by and large
far from the ideal (Fig. 2). Laser–tissue responses have been
described as an interaction between the sum of the qualities
of the laser beam and the target tissues. Because of the
variation in intensity distribution by the laser beam
(Fig. 2), the laser-to-enamel surface interaction can produce
irregular physical effects. These effects include untouched
enamel, subablative carbonate changes with superficial acid
resistance tendency, micro-exploded surfaces, and molten
enamel (Fig. 3).
According to Meister et al., effects of the transversal
mode profile can manifest themselves in the uneven spatial
distribution of optical intensity within the laser beam on the
sample surface, which can in turn create local and multiple
high peak power and high surface temperature spikes, or
“hot spots” [34]. It was reported that the Er:YAG laser
irradiation of enamel with 7 J/cm2 and a pulse duration of
150 μs could produce an average temperature spike of

Table 4 Predominant failure patterns (in percent) by stereomicroscope under ×40 magnification

Failure patterns Enamel surface preparations

AE+G5 LEAE+G5 LEAE-H+G5 G7 LE+G7

Adhesive 18 8 8 50 38
Mixed 82 62 69 50 62
Cohesive (resin) 0 15 0 0 0
Cohesive (enamel) 0 15 23 0 0

AE acid etch, LE laser etch, LEAE laser etch and acid etch, LEAE-H laser etch with higher pulse energy and acid etch, G5 and G7 recognized
generations of bonding resin, Adhesive complete adhesive failure at the interface between the bonding resin and enamel, Mixed partial adhesive
failure at the interface and partial cohesive failure within the bonding structure itself, Cohesive (resin) complete cohesive failure within the
composite structure, Cohesive (enamel) partial cohesive failure within the enamel substrate
Lasers Med Sci (2013) 28:879–889 885

Table 5 Adhesion studies of etch-and-rinse bonding resins and laser etch on enamel

First author Publication year Erbium laser Pulse energy Generation of bonding Statistical analysis
(beam profile) (energy density) resin (trade name)

Present study Er:YAG (CT) 40 mJ (14 J/cm2) 4th (New and Bond Photo Bond) LEAE0AE
5th (Prime & Bond NT) LEAE>AE
170 mJ (60 J/cm2) 5th (Prime & Bond NT) LEAE<AE
Lin 1998 Er,Cr:YSGG (CT) 300 mJ (68 J/cm2) 4th (XR Bond) LEAE0AE
De Munck 2002 Er:YAG (CT) 120 mJ (24 J/cm2) 4th (Optibond) LEAE<AE
Otsuki 2002 Er:YAG (FB) 200 mJ (52 J/cm2) 4th (Clearfil SE) LEAE>LE
Goncalves 2003 Er:YAG (FB) 80 mJ 5th (Single Bond) LEAE0AE
Lee 2003 Er:YAG (CT) 300 mJ (106 J/cm2) Orthodontic resin LE>LEAE, LE>AELE
Trajtenberg 2004 Er:YAG (CT) 260 mJ 4th (Scotch Bond) LEAE<AE
Dunn 2004 Er:YAG (CT) 240 mJ (85 J/cm2) 4th (Scotch Bond) LEAE<AE
Wanderley 2005 ER:YAG (FB) 60–100 mJ 5th (Single Bond) LEAE>AE (60–80 mJ),
LEAE0AE (100 mJ)
Marraccini 2006 Er:YAG 80 mJ (26 J/cm2) 5th (Single Bond) LEAE0AE
Lessa 2007 Er:YAG (FB) 80 mJ (28 J/cm2) 5th (Single Bond) LEAE0LE
Sasaki 2008 Er:YAG (FB) 80 mJ 5th (Single Bond) LEAE>LE, LEAE>AE
Firat 2010 Er:YAG (FB) 120 mJ (61 J/cm2) 5th (XP Bond) LEAE>AE (50 μs),
LEAE0AE (100 μs),
LEAE<AE (150, 300 μs)

Some of the laser parameters were calculated from information obtained from the studies; please refer to the original study for their precise settings,
especially for the related statistical analysis and conclusions
CT contact tip; FB free beam; 4th, 5th fourth or fifth generation of bonding resin; AE acid etch; LE laser etch; AELE acid etch laser etch
combination; LEAE laser etch acid etch combination; <, 0, > bond strength comparisons

∼300 °C and, at 9 J/cm2, an average surface temperature rise
of ∼1,000 °C [35]. Regarding the enamel substrate, the OH−
group is a key component of the hydroxyapatite crystal.
This group happens to have a separate absorption peak at
2.78 μm away from free water. Once free water is exhausted
after the initial photothermal explosions and cavitation
effects, it is quite possible that there is either inadequate or
nonexistent water rehydration at these spots of high optical
intensity created by the inhomogeneous beam profile; the
dominant optical absorption can be shifted to the intrinsic
water bound to apatite crystals and these OH− groups of the
mineral apatite. With a thermal relaxation time of about
90 μs for enamel [36], instead of water-mediated micro-
explosions, molten surface globules of enamel can be

Fig. 3 SEM photograph of the ablation on dental enamel by a single

Fig. 2 Multimode beam profile of the Er:YAG laser in this study laser pulse with TEM31 mode at a pulse energy of 50 mJ exemplifies its
captured by a pyroelectric camera (Pyrocam III by Spiricon, USA) uneven laser–tissue interactions
886
Fig. 4 Stereomicrograph of
enamel surfaces. a Surface
etched with 38 % phosphoric
acid. b Same acid-etched
enamel surface covered with
bonding resin
created by the absorption of this excess localized high peak
converted thermal power once the temperature increase
exceeds the melting point of enamel [37]. Ying et al. have
reported the presence of these melting and recrystallization
areas in enamel and suggested that the less permeable,
hypermineralized enamel surface could affect the enamel's
acidic resistance and hamper the subsequent wetting and
penetration of adhesive materials [38]. Such physical sur-
face changes of melting and recrystallization with the for-
mation of pores and molten globules of enamel have also
been reported in several studies [19, 25, 38–43]. The for-
mation of localized fused or molten enamel will increase the
surface tension, resist the spreading of phosphoric acid,
reduce the effectiveness of creating microporosities, and
hinder the penetration of the methacrylate monomers, result-
ing in the reported lower bond strength.
To avoid the possibilities of these excessive thermal
effects, we have kept the operating energy density at 14 J/
cm2, as close to the ablation threshold of enamel of 9–12 J/
cm2 [8] as possible. The under-hydration possibility was
further reduced by utilizing a relatively high irrigation rate
of 90 mL/min. When we brought the pulse energy and
energy density up to 170 mJ and 60 J/cm2, respectively,
which is comparable to most published studies (Table 5),
our bond strength results went down significantly. Using a
similar fifth-generation bonding resin, these detrimental
Fig. 5 Stereomicrograph of
enamel surfaces. a Surface
etched with laser (energy
density of 14 J/cm2). b Same
laser-etched enamel surface
covered with bonding resin
Lasers Med Sci (2013) 28:879–889
effects were also reported by Wanderly et al. in 2005 [44].
The loss in bond strength can also be explained with photo-
graphs taken with a stereomicroscope (×40 objective, Leica
MZ6 from Leica Microsystems GmbH, Wetzlar, Germany).
Figure 4a illustrates the buccal surface of a lower molar acid
etched with the same 38 % phosphoric acid as in this study,
and Fig. 4b shows the same surface covered with bonding
resin G5. Figure 5a illustrates the buccal surface of a similar
lower molar laser conditioned with the same energy density
of 14 J/cm2 as in this study. The optical appearance in
Fig. 5b is very similar to Fig. 4b when the same bonding
resin was applied. However, when the same higher energy
density of 60 J/cm2 was applied in Fig. 6a, the uneven
thermal effects were more extensive. From the remaining
opacities shown in Fig. 6b, it can be seen that the molten
enamel increased the surface tension and decreased the
surface area for adhesive impregnation, negatively affecting
the bond strength as demonstrated by the results in group
LEAE-H+G5 (Table 3).
Even though the ablation threshold of enamel was initially
published in 1989 [8], most of the published studies engaged
in much higher energy densities than 11 J/cm2 (Table 5).
Higher energy concentration—through the different beam
profile of a free beam or contact tip—may further exaggerate
the local peak temperature and hydration differences result-
ing in more patches of molten enamel than microexplosions.
Lasers Med Sci (2013) 28:879–889 887

Fig. 6 Stereomicrograph of
enamel surfaces. a Surface
etched with laser (energy
density of 60 J/cm2). b Same
laser-etched enamel surface
covered with bonding resin

This may explain the same white spots or molten enamel
globules (Fig. 6a) as observed by many authors and why
their higher pulse energy setting did not result in higher bond
strength as in our experiments. In the context of excessive
thermal alteration of the enamel surface, reduction of super-
ficial microporosities, and inhibition of subsequent penetra-
tion of bonding resin, the appearance of these clusters of
opacity at the enamel surface (Fig. 6b) may serve as an early
optical warning of impending poor resin integration, result-
ing in potential less than the ideal bond strength.
The addition of laser conditioning did not significantly
improve the adhesion for self-etch bonding resins G6 and G7
in our study (Table 3). Although it was suggested that the
removal of the smear layer and its related buffering effects by
laser irradiation could be beneficial for some weaker self-
etch adhesives [31], the improved surface roughness in gen-
eral did not translate into better resin interaction or bond
strength in many of the related studies (Table 6). On top of
the possibility of excessive thermal effects, the type of resin
chemistry in the sixth and seventh self-etch bonding resins
may not be suitable for the enamel surface after laser irradi-
ation [45] since the thermal alteration from laser condition-
ing may simply render some of the enamel surface slightly
more acid resistant, which may limit the conditioning effec-
tiveness of the weaker acids of these self-etch systems [32].
From our use of the energy density of 14 to 107 J/cm2
reported in literature (Table 6), the use of laser conditioning
in this range of energy densities apparently was not enough
to improve the enamel surface for the subsequent deminer-
alization and infiltration of the self-etch bonding resin.
The surface effects by laser conditioning depend heavily
on parameters such as energy density, pulse duration, expo-
sure time, irradiation distance, and water rehydration rate
[34–36, 38, 41, 42]. From our bond strength experiments
with a lower pulse energy setting of 40 mJ, the use of laser
conditioning was investigated as a possible adjunct for the
improvement of adhesion at the enamel surface. The use of
energy that is much higher than the enamel ablation

Table 6 Adhesion studies of self-etch bonding resins and laser etch on enamel

First author Publication year Erbium laser Pulse energy Generation of bonding Statistical
(exit profile) (energy density) resin (trade name) analysis

Present study Er:YAG (CT) 40 mJ (14 J/cm2) Futurabond DC, SE0LESE,

Futurabond NR SE0LESE
Miyazaki 2002 Er:YAG (CT) 200 mJ (70 J/cm2) 6th (Fluoro Bond) SE0LESE
Delfino 2007 Er:YAG (FB) 250 mJ (45 J/cm2), 6th (Tyrian SPE) SE>LESE
300 mJ (54 J/cm2)
Esteves-Oliverira 2007 Er:YAG (FB), 350 mJ (20 J/cm2), 6th (Clearfil SE) SE>LESE,
Er,Cr:YSGG (CT) 125 mJ (16 J/cm2) SE>LESE
Kemeyama 2008 Er:YAG (CT) 160 mJ (56 J/cm2) 6th (Clearfil Megabond), SE0LESE
7th (AQ Bond Plus,
G-Bond, Clearfil Tris Bond)
Cardoso 2008 Er,Cr:YSGG (CT) 300 mJ (107 J/cm2) 6th (Clearfil SE, SE>LESE (6th),
Adper Prompt-L-Pop), SE0LESE (7th)
7th (Clearfil S3 Bond)

Some of the laser parameters were calculated from information obtained from the studies; please refer to the original study for their precise settings,
especially for the statistical analysis and conclusions
CT contact tip; FB free beam; 6th, 7th sixth or seventh generation of bonding resin; SE self etch; LE laser etch; <, 0, > bond strength comparisons
888
thresholds may facilitate the ablation of enamel and dentin,
which maximizes the efficiencies of cavity preparation, but
the higher energy settings can amplify the unwanted thermal
effects, which results in lower bond strengths at the enamel
surface and thermal damage to the enamel and dentin sub-
strates. A lower energy setting may produce a relatively
even laser-conditioned enamel surface, less thermal dentinal
damage, and possibly better bond strength, but slower abla-
tion. To improve the enamel adherent surface through laser
irradiation, there appears to be a need to orchestrate this
group of laser parameters and manipulate their effects within
a relatively narrow periphery. The different wetting ability
or surface tension of these different patches of surface
patterns will dictate the different resin penetration and ad-
hesion; ultimately, all the qualities of these different effects
in conjunction will determine the final bond strength.
Conclusion
1. Based on the findings of this study and given the lim-
itations of an in vitro study, the addition of laser condi-
tioning at an energy density comparable to the ablation
threshold of enamel did significantly improve the bond
strength of the fifth generation of bonding resin. The
same additional laser conditioning did not significantly
change the bond strength of the fourth, sixth, and sev-
enth generations of bonding systems.
2. The use of a laser energy density close to the ablation
threshold of enamel had no detrimental effect on the
bond strength of the four groups of bonding resins
investigated when compared to similar published
results.
3. The use of laser energy density comparable to published
studies did significantly lower the bond strength of the
fifth generation of bonding resins. Most of the published
studies, including those that were not cited, involved
energy densities much higher than the ablation threshold
of enamel. The degraded enamel surface created and
ensuing poor bond strength results may be caused by the
combined excessive laser thermal side effects.
4. In addition to the surface effects by laser parameters
such as beam profile, pulse energy, and pulse duration
during laser conditioning, there is a need to include the
viscosity and wettability of the bonding system in fur-
ther bond strength studies.
Acknowledgments The authors wish to thank Mr. Franz Jungwirth
and Mrs. Patricia Buttler-Bücher of the University Hospital of Aachen
for their assistance in bond strength testing and stereo microscopy
image collection, respectively, and Mr. Eric Yung and Mr. Patrick Yung
for their active participation and support during sample collection and
preparation.
Lasers Med Sci (2013) 28:879–889
References
1. Baier R (1992) Principles of adhesion. Oper Dent (Suppl 5):1–9
2. Marshall SJ, Bayne SC, Baier R, Tomsia AP, Marshall GW (2010)
A review of adhesion science. Dent Mat 26:e11–e16
3. Hinoura K, Setcos JC, Philip RW (1988) Cavity design and place-
ment techniques for class 2 composites. Oper Dent 13(1):12–19
4. Buonocore MG (1955) A simple method of increasing the adhe-
sion of acrylic filling materials to enamel surfaces. J Dent Res
34:158–161
5. Boyde A, Jones SJ, Reynolds PS (1978) Quantitative and qualita-
tive studies of enamel etching with acid and EDTA. Scanning
Electron Microsc 2:991–1002
6. Maijer R, Smith DC (1986) Crystal growth on the outer enamel
surface—an alternative to acid. Am J Orthod 89:183–193
7. Ramos R, Chimello D et al (2002) Effect of Er:YAG laser on bond
strength to dentin of a self-etching primer and two single-bottle
adhesive systems. Lasers Surg Med 31:164–170
8. Hibst R, Keller U (1989) Experimental studies of the application of
Er:YAG laser on dental hard substances: I. Light microscopic and
SEM investigations. Lasers Surg Med 9:338–344
9. Sasaki KM, Aoki A, Ichinose S, Ishikawa I (2002) Ultrastructural
analysis of bone tissue irradiated by Er:YAG laser. Laser Surg Med
31(5):79–85
10. Aoki A, Ishikawa I, Yamada T, Otsuki M et al (1998) Comparison
between Er:YAG laser and conventional technique for root caries
treatment in vitro. J Dent Res 77(6):1404–1414
11. Cozean CD, Arcoria CJ, Pelagalli J, Powell GL (1997) Dentistry
for the 21st century? Erbium:YAG laser of teeth. J Am Dent Assoc
128:1080–1087
12. Staninec M, Gardner AK, Le CO, Sarma AV, Fried D (2006)
Adhesion of composite to enamel and dentin surfaces irradiated
by IR laser pulses of 0.5–35 μs duration. J Biomed Mater Res B
Appl Biomater 79:193–201
13. Hossain M, Yamada Y, Nakamura Y, Murakami Y, Tamaki Y,
Matsumoto K (2003) A study on surface roughness and micro-
leakage test in cavities prepared by Er:YAG laser irradiation and
etched bur cavities. Lasers Med Sci 18:25–31
14. Staninec M, Xie J, Le CQ, Fried D (2003) Influence of an optically
thick water layer on the bond-strength of composite resin to dental
enamel after IR laser ablation. Lasers Surg Med 33:264–269
15. Özer T, Başaran G, Berk N (2008) Laser etching of enamel for
orthodontic bonding. Am J Orthod Dentofacial Orthop 134:193–
197
16. Wigdor H, Abt E, Ashrafi S, Walsh JT Jr (1993) The effects of
lasers on dental hard tissues. J Am Dent Asso 124(2):65–70
17. Takamori K (2000) A histopathological and immunohistochemical
study of dental pulp and pulpal nerve fibers in rats after cavity
preparation using Er:YAG laser. J Endod 26(2):95–99
18. Armengol V, Jean A, Rohanizadeh R, Hamel H (1999) Scanning
electron microscopic analysis of diseased and healthy dental hard
tissues after Er:YAG laser irradiation: in vitro study. J Endo 25
(8):543–546
19. Freitas PM, Navarro RS, Barros JA, Eduardo CP (2007) The use of
Er:YAG laser for cavity preparation: an SEM evaluation. Microsc
Res Tech 70:803–808
20. Délme KI, De Moor RJ (2007) Scanning electron microscopic
evaluation of enamel and dentin surfaces after Er:YAG laser prep-
aration and laser conditioning. Photomed Laser Surg 25:393–401
21. Armengol V, Laboux O, Weiss P, Jean A, Hamel H (2003) Effects
of Er:YAG and Nd:YAP laser irradiation on the surface roughness
and free surface energy of enamel an dentin: an in-vitro study.
Oper Dent 28(1):67–74
22. De Munck J, Van Meebeek, Yudihira R, Lambrechts P, Vanherle G
(2002) Micro-tensile bond strength of two adhesives to erbium:
Lasers Med Sci (2013) 28:879–889
YAG-lased vs. bur-cut enamel and dentin. Eur J Oral Sci 110:322–
329
23. Martinez-Insua A, da Silva Dominguez L, Rivera FG, Santana-Penin
UA (2000) Differences in bonding to acid-etched or Er:YAG-laser-
treated enamel and dentin surfaces. J Prosthet Dent 84(3):280–288
24. Chimello-Sousa DT, de Souza AE, Chinelatti MA, Pecora JD,
Palma-Dibb RG, Corona SAM (2006) Influence of Er:TAG laser
irradiation distance on the bond strength of a restorative system to
enamel. J Dentist 34:245–251
25. Goncalves M, Corona SA, Borsatto MC, Silva PCG, Pacora JD
(2003) Influence of the frequency of Er:YAG laser on the bond
strength of dental enamel. J Clin Laser Med Surgery 2:105–108
26. Attrill DC, Farrar SR, King TA, Dickinson MR, Davies RM,
Blinkhorn AS (2000) Er:YAG (λ02.94 μm) laser etching of
dental enamel as an alternative to acid etching. Lasers Surg
Med 15:154–161
27. Low T, Lee KW, von Fraunhofer JA (1978) The adaptation of
composite materials to etched enamel surfaces. J Oral Rehabil
5:349–355
28. Apel C, Meister J, Ioana RS et al (2002) The ablation threshold of
Er:YAG and Er:YSGG laser radiation in dental enamel. Lasers
Med Sci 17:246–252
29. Øilo G (1993) Bond strength testing—what does it mean? Int Dent
J 43:492–498
30. Finger WT, Fritz UB (1997) Resin bonding to enamel and dentin with
one-component UDMA/HEMA adhesives. Eur J Oral Sci 105:183–186
31. Shinchi MJ, Soma K, Nakabayashi N (2000) The effect of phos-
phoric acid contraction on resin tag length and bond strength of a
photo-cured resin to acid-etched enamel. Dent Mater 16:324–329
32. Eguro T, Maeda T, Tanabe M, Otsuki M, Tanaka H (2001) Adhe-
sion of composite resins to enamel irradiated by the Er:YAG laser:
application of the ultrasonic scaler on irradiated surface. Laser
Surg Med 28(4):365–370
33. Obeidi A, McCracken M, Liu PR, Litaker MS, Beck P, Rahemtulla
F (2009) Enhancement of bonding to enamel and dentin prepared
by Er, Cr:YSGG laser. Laser Surg Med 41(6):454–462
34. Meister J, Franzen R, Apel C, Gutknecht N (2004) Influence of the
spatial beam profile on hard tissue ablation part II: pulse energy
889
and energy density distribution in simple beams. Lasers Med Sci
19:112–118
35. Seka W, Featherstone JD, Fried D, et al. (1996) Proceedings of
SPIE—the International Society for Optical Engineering.
2672:144–158
36. Fried D, Zuerlein M, Featherstone JDB, Seka W, Duhn C,
McCormack SM (1998) IR laser ablation of dental enamel:
mechanistic dependence on the primary absorber. Appl Surf
Sci 127–129:852–856
37. Meister J, Franzen R, Forner K, Grebe H, Stanzel S, Lampert F,
Apel C (2006) Influence of the water content in dental enamel and
dentin on ablation with erbium YAG and erbium YSGG lasers. J
Biomed Optics 11(3):034030-1–7
38. Ying D, Chuah GK, Hsu CYS (2004) Effect of Er:YAG laser and
organic matrix on porosity changes in human enamel. J Dent
32:41–46
39. Sato K (1983) Relation between acid dissolution and histological
alteration of heated tooth enamel. Caries Res 17:490–495
40. Burkes EJ, Hoke J, Gomes E, Wolbarsht M (1992) Wet versus dry
enamel ablation by Er:YAG laser. J Prosthet Dent 67:845–851
41. Delfino CS, Souza-Zaroni WC, Corona SAM, Palma-Dibb RG
(2006) Effect of Er:YAG laser energy on the morphology of
enamel/adhesive system interface. Appl Surf Sci 252(24):8476–
8481
42. Hossain M, Nakamura Y, Yamada Y, Kimura Y, Nakamura G,
Matsumoto K (1999) Ablation depths and morphological changes
in human enamel and dentin after Er:YAG laser irradiation with
and without water mist. J Clin Laser Med Surg 17:105–109
43. Souza-Gabriel AE, Chinelatti MA, Borsatto MC, Pecora JD,
Plama-Dibb RG, Corona SAM (2008) SEM analysis of enamel
surface treated by Er:YAG laser: influence of irradiated distance.
Microsc Res Tech 71:536–541
44. Wanderley RL, Monghini EM, Pecora JD et al (2005) Shear bond
strength to enamel of primary teeth irradiated with varying Er:
YAG laser energies and SEM examination of the surface morphol-
ogy: an in vitro study. Photomed Laser Surg 23(3):260–267
45. Camps J, Pashley DH (2000) Buffering action of human dentin in
vitro. J Adhes Dent 2(1):39–50