Lasers in Surgery and Medicine 27:111–118 (2000)

Sealant Bond Strengths of CO2 Laser-Etched

Versus Acid-Etched Bovine Enamel
James L. Drummond, DDS, PhD,1* Harvey A. Wigdor, DDS,2 Joseph T. Walsh, Jr., PhD,3†
Shahrbanoo Fadavi, DDS, MS,4 and Indru Punwani, DDS, MS4
1
Department of Restorative Dentistry, University of Illinois at Chicago, Chicago, Illinois
2
Ravenswood Hospital Medical Center, Chicago, Illinois
3
Biomedical Engineering Department, Northwestern University, Evanston, Illinois
4
Department of Paediatric Dentistry, University of Illinois at Chicago, Chicago, Illinois

Background and Objective: The purpose of this study was to evaluate

sealant shear bond strength on bovine enamel with standard acid etch-
ing compared with CO2 laser etching.
Study Design/Materials and Methods: Bovine enamel was prepared ei-
ther by acid or laser etching and divided into four experimental
groups, either acid or laser-etched teeth with or without a primer. A
gelatin capsule was used to place the sealant on the prepared enamel
surface and the bond tested in shear. Also surface roughness was evalu-
ated by using a surface analyzer and an atomic force microscope.
Results: Shear bond strength results were the following: acid etch = 8.8
± 3.8 MPa, acid etch with primer = 10.3 ± 5.5 MPa, laser etch = 4.0 ± 1.1
MPa, and laser etch with primer = 6.2 ± 2.3 MPa. Analysis of variance
statistical analysis found no significant difference in bond strength
between the acid-etched groups. However, the laser-etched groups had
significantly lower bond strengths from the acid-etched teeth. In addi-
tion, a significant difference was observed between the laser-etched
groups, where the use of the primer helped to increase the bond
strength of the sealants. The surface roughness was significantly
greater on the laser-etched teeth at the mm level (by using a surface
analyzer) from the acid-etched and the control specimens. No differ-
ence in roughness (by using an atomic force microscope) was observed
at the nanometer level between the laser and acid-etched teeth.
Conclusion: For these particular settings, the laser-etched teeth re-
sulted in lower bond strengths to enamel and the use of a primer in-
creased the bond strength for laser-etched teeth only. Lasers Surg.
Med. 27:111–118, 2000. © 2000 Wiley-Liss, Inc.

Key words: laser and acid etching; enamel bond strength

INTRODUCTION ment, but no change in retention was observed

Sealants have been used as a preventive
measure for over 30 years; however, increased re-
tention time of sealants continues as a research
focus [1]. One approach to increase retention has
been the use of bonding agents [2,3]. When used
in a moist environment, primers (one component
of bonding agents), have increased the sealant
bond strength [4].
Recently, instead of acid etching, lasers have
been used for etching of the enamel surface. Ar-
coria et al. used a CO2 laser to produce a surface
roughness similar to that of an acid etch treat-
[5]. Walsh et al. found that the shear strength of
resin was higher for CO2 laser-etched samples
than traditional acid etch samples [6]. Corpas-
Pastor et al. examined the tensile bond strength
of orthodontic brackets between acid-etched and
†
In accordance with the policy of the Journal, the designated
author discloses a financial or other interest in the subject
discussed in this article.
*Correspondence to: James L. Drummond, DDS, PhD, 337A
College of Dentistry (m/c 555), 801 South Paulina, University
of Illinois at Chicago, Chicago, IL 60612-7212.
E-mail: drummond@uic.edu
Accepted 25 February 2000

© 2000 Wiley-Liss, Inc.

112 Drummond et al.
laser-etched teeth after thermal cycling and found TABLE 1. Surface Preparation of the Bovine Teeth
that the acid-etched teeth had significantly Group Code Procedure
higher bond strength [7]. Bouvier et al. examined
One AE Acid etch + sealant
the effect of lased dentin versus unlased dentin Two AEP Acid etch + primer + sealant
and found the tensile bond strength of unlased Three LE Laser etch + sealant
dentin was significantly higher [8]. Shahabi et al. Four LEP Laser etch + primer + sealant
found no difference in shear bond strength on hu-
man enamel for CO2 lased versus unlased sur-
faces [9,10]. Ariyaratnam et al., by using a TABLE 2. Static Shear Bond Strength† (MPa ± SD)
Nd:YAG laser, found all lased teeth to have sig-
nificantly lower bond strength than the acid- Group N Bond strength Significance*
etched teeth [11]. Enamel surfaces treated with a AE 32 8.8 ± 3.8 A
laser also develop more resistance to caries for- AEP 30 10.3 ± 5.5 A
LE 30 4.0 ± 1.1 C
mation [12]. The inconclusive results from the la- LEP 35 6.2 ± 2.3 B
ser etching of teeth with respect to bond strength
were the impetus for the present study. P values for Tukey analysis of shear bond strength
Many different types of lasers exist, and pro-
AE AEP LE LEP
duce different results on dental hard tissue
AE 1.000
[13,14]. Some CO2 lasers are able to operate at a
AEP 0.301 1.000
lower radiant exposure, compared with other la- LE 0.000 0.000 1.000
sers, because of the efficient transfer of optical LEP 0.019 0.000 0.050 1.000
energy to heat in enamel and dentin. This effi- †
AE, acid etched plus sealant; AEP, acid etched plus primer
ciency is accomplished because of the greater ab- plus sealant; LE, laser etched plus sealant; LEP, laser etched
sorption in the hydroxyapatite component of the plus primer plus sealant.
dental hard tissues in the wavelength range from *Groups with same letter were not statistically significant at
9.3 to 9.8 mm. the 0.05 level.
The intent of this project was to evaluate the
shear bond strength on bovine enamel between mounted teeth were stored in distilled water at
acid-etched teeth and laser-etched teeth with and room temperature.
without a primer. A CO2 laser-emitting short A prototype CO2 laser (Laser Industries, Tel
pulses at radiation was used to etch the enamel Aviv, Israel) that emits 9.6-mm radiation, strongly
with limited thermal alteration of the surface. absorbed by the hydroxyapatite of the bovine
Surface roughness was evaluated and microscopy enamel was used at a power setting of 3.5 watts.
examination carried out by using a scanning elec- The laser emitted a series of 20 mJ, 60-ms-long
tron microscope and an atomic force microscope. pulses focused to approximately a 250-mm-
diameter spot on the enamel surface. The spot
was mechanically scanned along a helical path to
MATERIAL AND METHODS
create a pattern of shallow ablation craters within
The roots of 128 bovine incisors without ob- a 2.5-mm-diameter circular area. The 2.5-mm-
vious defects, caries, or attrition were removed diameter area was then manually scanned over
leaving only the clinical crowns, which were an approximately 8-mm-diameter area to achieve
stored in room temperature, distilled water. Dis- an etch. To minimize the accumulation of thermal
tilled water was chosen as the storage medium energy, a compressed nitrogen gas/water mixture
because a previous study by Goodis et al. indi- was sprayed on the surface of the tooth at a rate of
cated no difference in shear strength strengths for ∼10 ml/min. These parameters were selected after
teeth stored in either 70% ethanol, 10% formalin, a extensive series of experiments, to achieve a
distilled water, or distilled water with thymol clinically acceptable etch rate while causing lim-
[15]. The extracted incisors were all prepared and ited damage to the remaining enamel.
tested within a time period of 3 months post mor- The tooth was covered with an aluminum
tem. The clinical crowns were embedded in auto mask 8 mm in diameter. The effective spot of the
polymerizing acrylic resin (Vitacrilic, Fricke Den- laser (2.5 mm) was swept along a linear raster
tal Manufacturing Company, Villa Park, IL) in a scan pattern inscribed in a square area of 8 mm
rubber mold. They were then randomly placed by 8 mm The sweep path followed a right/down/
into four different groups (see Table 1). All left/down pattern, originating in the top left cor-
 Bond Strengths of CO2 Laser-Etched Versus Acid-Etched Enamel 113
TABLE 3. Surface Roughness†

Surface analyzer Ra* t-Test AFM Ra

Group N (mm ± SD) P value* (nm ± SD) Significance*
Control parallel (CPA) 5 0.46 ± 0.23 A 0.042 13.04 ± 2.72 A
Control perpendicular (CPE) 5 1.12 ± 0.56 AB
AE parallel (AEPA) 6 1.87 ± 0.36 B 0.027 77.41 ± 23.80 B
AE perpendicular (AEPE) 5 2.45 ± 0.37 BC
LE parallel (LEPA) 6 4.83 ± 1.04 D 0.053 64.74 ± 15.23 B
LE perpendicular (LEPE) 6 3.82 ± 1.22 CD

P values for Tukey analysis of shear bond strength

CPA CPE AEPA AEPE LEPA LEPE

CPA 1.000
CPE 0.742 1.000
AEPA 0.050 0.588 1.000
AEPE 0.004 0.092 0.795 1.000
LEPA 0.000 0.000 0.000 0.000 1.000
LEPE 0.000 0.000 0.002 0.059 0.225 1.000
†
AE, acid etched; LE, laser etched; AFM, atomic force microscope.
*Groups with same letter were not statistically significant at the 0.05 level. The t-test was between parallel and perpendicular
surface within each group.

Fig. 1. Bovine enamel control.

114 Drummond et al.
Fig. 2. Bovine enamel after acid etching.
ner of the square, and ending in the bottom right
corner. To ensure homogeneity of the etch, the
path was then reversed, tracing a left/up/right/up
trajectory inside the square. The total scan was
composed of 14 passes (7 down and 7 up) in 12–13
seconds. The average effective etch time (within
the mask) was 8–10 seconds. The continuous lin-
ear scan, combined with the helical motion of the
focus, ensured a homogeneous, stochastic etch.
The use of the mask resulted in a sharp transition
form etched to nonetched surfaces.
The sealant used (Aelite Seal, Bisco Dental
Products, Itasca, IL) was a dual-cured pit and fis-
sure sealant composed of bisphenol diglycidyl-
methacrylate with amorphous silica, titanium di-
oxide, and benzoyl peroxide (catalyst). The primer
was made of ethyl alcohol and hydroxyethyl meth-
acrylate. The bonding procedures given by the
manufacturer’s instructions were as follows.
Acid Etching Without Primer
The enamel surface was cleaned with a rub-
ber cup and pumice for 15 seconds; dried with oil
free, moisture free, compressed air for 5 seconds;
etched with 37% phosphoric acid gel (Bisco Dental
Products) placed with a syringe needle tip;
washed for 10 seconds with distilled water; and
then dried with oil-free compressed air until
chalky white. A gelatin capsule 4.34 mm in diam-
eter (#5, Eli Lilly and Co., Indianapolis, IN) was
filled with the dual curing sealant and bonded to
the prepared tooth and cured for 20 seconds by
using a visible light curing unit (Visiluxll, 3M,
Minneapolis, MN). The bonded tooth was then
stored in room temperature distilled water.
Acid Etching With Primer
The enamel surface was treated as above ex-
cept for the final drying step. Instead of drying
with compressed air, the etched enamel surface
was kept moist by using a wet facial tissue
(Kleenex Softique, Kimberly-Clark Corporation,
Neenah, WI) to remove only the excess water. The
method of maintaining the moist surface had no
effect on the bond strength as observed in a pre-
vious study [4]. Two coats of primer were added to
 Bond Strengths of CO2 Laser-Etched Versus Acid-Etched Enamel
Fig. 3. Bovine enamel after laser etching.
the surface of the enamel as per manufacturer’s
instructions. The enamel surface was dried with
oil-free compressed air for 10 seconds and then a
gelatin capsule, as above bonded to the surface.
Laser Etching Without Primer
The enamel surface was cleaned with a rub-
ber cup and pumice for 15 seconds and then
etched by using the CO2 laser as described above.
The etched samples were stored in a 100% humid
environment for 12 hours (half an inch of 2 × 2
nonsterile wet gauze was placed at the bottom of
the container and the etched tooth were placed on
top of the wet gauze). The etched surface was then
washed for 10 seconds with distilled water; dried
with oil-free compressed air until chalky white,
and a gelatin bonded to the surface. The bonded
tooth was then stored in room temperature dis-
tilled water. The 12-hour storage time was re-
quired because the laser was not housed at the
same place as the bonding and testing procedures
and travel time was required.
115
Laser Etch With Primer
The enamel surface was prepared the same
as the laser-etched and primer placed as above by
using a moist surface. The gelatin capsule was
bonded, and the specimens were stored at room
temperature in distilled water.
All of the bonded teeth were stored at room
temperature in distilled water for 7 days before
the shear bond strength test was completed.
Shear bond strength was completed on a material
testing machine (Instron 1152, Instron Corp.,
Canton, MA) at a crosshead speed of 2 mm/min.
The bond strength was determined by dividing
the load at fracture by the sealant area.
Surface roughness (Ra) measurements (1
mm in length) were made on an unaltered bovine
incisor, an acid-etched bovine incisor, and a CO2
laser-etched bovine incisor by using a Surftest
201 surface analyzer (Miutoyo Manufacturing
Co., Ltd., Tokyo, Japan). Roughness was mea-
sured parallel and perpendicular to the long axis
of the tooth to compensate for the dominant ridges
parallel to the long axis of the tooth. To measure
116 Drummond et al.
Fig. 4. Cross-section of bovine enamel after laser etching.
the surface roughness at a much smaller scale, an
atomic force microscope was used (ARIS-3300
Personal Atomic Force Microscope, Burleigh In-
struments, Inc., Fisher NY) with line scans 1.4
mm in length.
Scanning electron microscopy (SEM) [JOEL
35C, JOEL USA, Peabody, MA] was completed for
the control, acid-etched, and laser-etched sur-
faces. The specimens were coated with gold-
palladium.
The statistical analysis for the bond strength
and surface roughness consisted of a one-way
analysis of variance followed by a Tukey multiple
means comparison test when required. For the
comparison between the parallel versus perpen-
dicular surface roughness within each material
(control, acid-etched, and laser-etched), a Stu-
dent’s t-test was used.
RESULTS
The shear bond strength and statistical
analysis are reported in Table 2. A significant dif-
ference existed between the acid-etched groups
and the laser-etched groups. The two acid-etch
groups were not significantly different from each
other; however, the laser-etched groups were sig-
nificantly different from each other.
Table 3 presents the result from the rough-
ness study. The statistical analysis showed that
the orientation of the tooth had an effect on the
measured roughness. The laser-etched surface
was the roughest followed by the acid-etched and
then the control. A t-test was then conducted be-
tween the orientation (parallel vs. perpendicular
to the long axis), showing that for both the control
and the acid-etched, there was a significant dif-
ference depending on orientation. For the laser-
etched tooth, there was no significant difference
in orientation. The roughness from the atomic
force microscope only showed a significant differ-
ence between the two etched surfaces and the con-
trol. The differences observed between the two
techniques are one of scale. The region measured
by the atomic force microscope is much smaller,
between the ridges, than the surface analyzer,
which crossed over the ridges, resulting in the in-
creased roughness.
 Bond Strengths of CO2 Laser-Etched Versus Acid-Etched Enamel
SEM photographs of the control, acid-etched,
and laser-etched surfaces are presented in Fig-
ures 1–4. Figure 1 is the unetched surface of bo-
vine enamel and Figure 2 is the surface after acid
etching. The surfaces presented were representa-
tive of the bovine enamel specimens. Figure 3 is
the laser-etched surface with crack formation in
the re-solidified enamel. No crack formation was
observed in any teeth outside of the region of the
laser etching. Figure 4 is a cross-section of the
laser-etched surface showing the depth effect of
the laser to be approximately 1–2 mm.
DISCUSSION
The results showed that for the parameters
used, laser etching on the bovine enamel pro-
duced a significantly lower bond strength. The
power settings that were used produced a laser-
etched, re-solidified enamel. The acid-treated
samples revealed a typical morphology observed
for acid-etched enamel. The decrease in bond
strength for the laser-etched teeth may not be a
function of surface roughness, but of the surface
energy of the etched surface. The acid etching pro-
cess leaves a high-energy surface that is easily
wetted by the sealant. The laser-etched surface on
the other hand, is most likely at a lower surface
energy because the surface was melted and then
re-solidified. Another possibility is that failure of
the bond occurred between the re-solidified
enamel and the unaltered enamel and not be-
tween the sealant and the enamel.
The laser-treated surface would also be ex-
pected to have a lower water content than the
original tooth, because the water and organic
phase of the tooth would be volatilized during the
laser etching. With less moisture on the surface,
the wetting properties of this acetone-based seal-
ant system are reduced, limiting sealant penetra-
tion into the enamel surface undercuts, and re-
sulting in the observed reduced bond strengths.
This idea is supported because both etched sur-
faces showed an increase in bond strength after
the use of the acetone based primer. The tooth
preparation technique provided a moist surface
and not an air-dried surface.
The higher surface roughness observed for
the laser-etched specimens at the micrometer
level did not translate into a higher bond
strength. The surface roughness at the micron
level is attributed to the prominent ridges present
on the surface of bovine teeth. At the atomic force
level of nanometers, the roughness was the same
117
between laser-etched and acid-etched teeth. Most
of literature states that a decrease in bond
strength is observed when enamel was laser-
treated, but Walsh et al. [6] noted that in their
study that a significant increase (P < 0.0001) in
bond strength is seen when enamel was laser
treated. It should be noted that these authors had
used numerous parameters (different power set-
tings) for their study and only one of nine showed
the greater bond strength, whereas all the others
showed a decrease in bond strength. Only one
power setting was used in our study to measure
shear bond strength and the effect of a primer and
additional research would be needed to determine
the most optimal setting, which would mimic the
characteristics of acid etching and improve the
sealant bond strength.
Research has shown that lasers can alter the
morphology of enamel to make it less susceptible
to caries. This finding may yet be a more practical
approach with regard to laser use in preventative
dentistry.
ACKNOWLEDGMENTS
The authors thank Yang-sun Bak for his as-
sistance in the sample preparation and testing,
the Research Resources Center at the University
of Illinois at Chicago, for the use of the scanning
electron microscope, and Laser Industries, Tel
Aviv, Israel, for use of the laser.
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