Experimental Mechanics
DOI 10.1007/s11340-015-0087-0
Effects of a Nano-composite Adhesive on Mechanical Properties
of Tooth Enamel After Removing Orthodontics Bracket –
an Experimental Study Using Nano-indentation Test
A. Karimzadeh 1 & M.R. Ayatollahi 1 & T. Hosseinzadeh-Nik 2
Received: 5 March 2015 / Accepted: 12 August 2015
# Society for Experimental Mechanics 2015
Abstract The purpose of this study is to investigate and com-
pare effect of bracket bonding-debonding by nano-composite
and composite adhesives on mechanical properties of tooth
enamel. Orthodontic brackets were bonded to the enamel sur-
face and the mechanical properties of tooth enamel were stud-
ied by nano-indentation technique after bracket removal.
Twenty human premolar teeth were prepared and divided into
two groups. In one group, orthodontic brackets were bonded
by a conventional composite adhesive and in the other group a
dental nano-composite was used for bonding the brackets on
the buccal surface of tooth enamel. The brackets were then
debonded with a sharp-edged debonding pliers. After
debonding the brackets, the teeth were sectioned transverse
to their longitudinal axes from the middle of the bracket bond-
ed regions. Nano-indentation experiments were performed on
the enamel section at two regions: intact enamel and under-
the-bracket enamel. Then mechanical properties of the enamel
at these two regions, including elasticity modulus, hardness
and fracture toughness were determined from the nano-
indentation test results for both types of adhesives. Using the
nano-composite decreases the magnitudes of elasticity modu-
lus and hardness of the dental enamel under the brackets sig-
nificantly in comparison with the conventional orthodontic
adhesives. However, no significant difference is seen between
* M. R. Ayatollahi
m.ayat@iust.ac.ir
1
Fatigue and Fracture Lab., Center of Excellence in Experimental
Solid Mechanics and Dynamics, School of Mechanical Engineering,
Iran University of Science and Technology, Tehran, Iran
2
Dental Research Center Dentistry Research Institute & Department
of Orthodontics, Faculty of Dentistry, Tehran University of Medical
Sciences, Tehran, Iran
the fracture toughness reductions due to the use of composite
and nano-composite adhesives.
Keywords Dental nano-composite adhesive . Bracket
bonding effect . Nano-indentation experiment . Mechanical
properties . Enamel
Introduction
Different methods are used for bonding brackets on the dental
enamel in orthodontics applications. These methods can affect
the mechanical properties of dental enamel. An appropriate
method of bracket bonding has sufficient bond strength to
resist in situ forces, while it causes minimum defect on the
tooth enamel. After orthodontics treatment, brackets should be
removed from the teeth enamel. There are also different
debonding methods for the brackets removal. However,
bracket bonding-debonding may cause enamel damage
[1–4]. Knowing the way and the amount that bracket
bonding-debonding affect the enamel properties helps ortho-
dontists for better understanding the possible types of failure
such as enamel fracture and also for selecting the appropriate
method of bracket bonding.
Recently, nanofillers with dimensions of less than 100 nm
have been added to dental composite resins for producing
dental nano-composites. The clinical use of nano-composite
adhesives needs information about the bond strength of
brackets bonded by them on the tooth enamel. Moreover, the
mechanical properties of new adhesives and their effects on
the dental enamel properties should be investigated. Previous
research studies have shown that dental nano-composites pos-
sess good mechanical and optical properties [5–8], seal
strongly to enamel and dentine [9] and their bond strength
values for the bracket bonding are more than the minimum

value of bond strength that has been recommended for suc-
cessful clinical bonding [10–13]. While a few studies have
been performed on the bond strength of dental nano-
composites in orthodontics applications, but their effects on
the mechanical properties of enamel after bracket removal
have not been studied, yet.
Considering the limitations of classical methods, the nano-
indentation method could be a suitable alternative for measur-
ing the mechanical properties in small samples like tooth [14,
15, 10]. This technique can be used for measuring properties
like elasticity modulus, hardness and fracture toughness. In the
present study, the effects of dental nano-composite adhesive on
the mechanical properties of dental enamel after bracket
debonding were investigated and were compared with those
of the conventional composites. The hypothesis is that bonding
the orthodontic brackets on tooth using the nano-composite
adhesive will reduce the damage of the enamel under the
bracket.
Materials and Methods
Sample Preparation
Twenty human premolar teeth, extracted for orthodontics rea-
sons, were collected and stored in distilled water at a temper-
ature below 4 °C. Water changed weekly to prevent dehydra-
tion and bacterial growth. The buccal surfaces of all teeth were
examined under stereomicroscope at a magnification of 10
times and any tooth with any large restoration or caries which
could affect the enamel strength was removed from the study.
Before bonding the brackets, all the teeth were cleaned and
polished with pumice and rubber cup for 15 s on a slow-speed
contra-angle hand piece and then rinsed thoroughly and dried.
A 37 % phosphoric acid gel (Chemidarou, Iran) was applied in
the middle of buccal surface for bonding the brackets and then
after 30 s the surface was rinsed for 30 s with water spray and
dried with an oil-free air source for 20 s. After surface prepa-
ration, all the teeth were divided randomly into two equal
groups.
In the first group, ceramic brackets (Clarity Metal-
Reinforced 6400-823, 3M Unitek, USA) were bonded with
the composite adhesive (Transbond XT, 3M Unitek, USA) on
the etched enamel of 15 teeth according to the following
stages. First, a thin film of Transbond XT primer was applied
to the enamel surface and the Transbond XT adhesive paste
was applied to the bracket base. Then, the bracket was posi-
tioned on the specified enamel surface and pressed firmly and
uniformly. The excess adhesive around the bracket was re-
moved with a dental scalar carefully, and then the adhesive
was light cured perpendicular to the bracket surface for 5 s, as
instructed by the manufacturer of composite adhesive.
Exp Mech
In the second group, the ceramic brackets were bonded
using the nano-composite adhesive (Filtek Z350 XT, 3M
ESPE, USA) to the teeth in the same way described for the
first group. According to the manufacturer’s instruction, any
primer used for bonding the composite adhesive is appropriate
for the nano-composite one too. Thus, in the second group, a
thin film of Transbond XT primer was applied to the enamel
and then Filtek Z350 XT nano-composite was applied to the
bracket base and the bracket was bonded at the middle of the
buccal surface. As instructed by the manufacturer, the nano-
composite adhesives were light cured for 20 s perpendicular to
the bracket surface.
After bonding the brackets, all the teeth were stored in
distilled water at the temperature of 37 °C. Then, the samples
were thermo-cycled in distilled water for 1000 cycles between
5 and 55 °C with dwell time of 50 s at each temperature, as
proposed by Gale and Darvell [16]. After thermo-cycling, the
samples were kept for 1 h in the ambient conditions at 23 °C
before bracket removal. All the brackets were debonded with
a sharp-edge bracket removal pliers (i00545, narrow; Rocky
Mountain Orthodontics, USA). The bonded brackets were
placed between the blades of the pliers in a mesiodistal direc-
tion at the bracket-adhesive interface because of the curvature
at the base of the premolar brackets.
After debonding all of the brackets, the teeth were cut
transverse to their longitudinal axes from lines AA and BB
shown in Fig. 1 to prepare samples for nano-indentation tests.
Then to obtain a smooth surface for nano-indentation test, the
surfaces of all samples were polished successively by dia-
mond pastes with mesh sizes of 1 and 0.5 μm. The roughness
values of samples were checked using atomic force microsco-
py (AFM).
Nano-indentation Experiment
In order to investigate the bracket bonding-debonding effects
on the enamel, nano-indentation experiment was applied on
the enamel under the bracket-bonding site and on the intact
enamel as a control place. The nano-indentation test was per-
formed by using Triboscope system (Hysitron Inc., USA) with
a Berkovich indenter and based the on ISO 14577 standard.
The tip of testing instrument was calibrated by Oliver-Pharr’s
method and the same method was used for analyzing the ex-
perimental data [17–19].
The nano-indentation experiment uses an established meth-
od in which an indenter tip is immerged into specific sites of
the material to be tested, by applying an increasing normal
load. When the penetration depth of the indenter tip reaches
a pre-set maximum value, the normal load is reduced to zero.
Following one cycle of loading and unloading, a hole with
nanometer dimensions is formed.
In the current study, the indentation load of 5000 μN with a
constant rate of 15 μN.s−1 was selected. Each indentation
Exp Mech
Fig. 1 Sample preparation
stages, a) tooth after bracket
debonding, the square on the
tooth shows the bracket base
region; b) a tooth sample cut for
nano-indentation experiment
experiment consisted of three steps: loading, holding the in-
denter at peak load for 10 s, and unloading completely. After
the unloading stage, the test samples were allowed to have
complete relaxation and then AFM images were taken from
each sample surface. Figure 2 illustrates sample AFM images
before and after the nano-indentation experiment. According
to the described method, at least three indentations on each
site of the samples were performed at a temperature of 24 °C.
Elasticity modulus
In the nano-indentation tests, the elasticity modulus of sample
material (E) can be calculated by using the Sneddon relation-
ship [20]:
1 1− ν2 1− ν2i
¼ þ ð1Þ
Eeff E Ei
where ν is the Poisson’s ratio of samples which is equal to
0.28 [21]. Ei and νi are the elasticity modulus and Poisson’s
ratio of the indenter tip which are equal to 1140 GPa and 0.07,
respectively, according to the technical data available for the
related Triboscope system. Eeff is the effective elasticity mod-
ulus of material obtained from the nano-indentation test by
using the Oliver-Pharr’s method.
According to the Oliver- Pharr’s method, the effective
modulus of elasticity is calculated from the slope of tangent
line on the unloading segment of load–displacement curve at
the maximum indentation load. The load-displacement curve
is obtained from a complete cycle of loading and unloading
during the nano- indentation test. A sample of this curve and
its tangent line has been shown in Fig. 3.
The AFM images of all indentation tests were studied and
the elasticity moduli of all samples for the enamel under the
bracket bonding site and for the intact enamel were calculated
by using equation (1) but only for those tests where no redial
cracks around the indentation hole were observed. The values
used for νi and Ei are based on the technical data available for
the related Triboscope system. It is noteworthy that the load–
displacement curves of each test sample obtained from the
nano-indentation technique demonstrated good repeatability
for the dental enamel at both tested areas. Figure 4 shows
the load-displacement curves obtained from
For investigating the bracket bonding-debonding effect on
the enamel properties, the difference between the elasticity
modulus values of the intact enamel and under-the-bracket
enamel was obtained for each sample.
Hardness
Material hardness is defined as the resistance of material
against surface deformation caused by an external load. This
mechanical property is calculated by dividing the normal load
by the projected area of the surface where load is imposed on.
The hardness or the normal hardness (Hn) was obtained
from the nano-indentation experiment. According to [17],
the hardness could be calculated in the nano-indentation test
from:
FN
Hn ¼ ð2Þ
A
where FN is the maximum indentation load and A is the
projected area of the contact surface between the specimen
and the indenter. In this study, for calculating FN and A in
equation (2), the load-displacement curve obtained from the
nano-indentation test and also the Oliver-Pharr method were
used [17].
Fracture toughness
As a measure of material resistance against crack growth,
fracture toughness is another property, which can be obtained
from the nano-indentation test results. For this purpose the
applied load should be such selected to generate at least one
 Exp Mech

Fig. 2 Samples of AFM images taken from specimen surface a) before nano-indentation and b) after nano-indentation

crack at the corners of indentation hole. When nano-
indentation tests are performed on brittle materials like enam-
el, fracture toughness can be calculated from [22, 23]:
rffiffiffiffiffi
E P
Kc ¼ α ð3Þ
H c 32
where P is the maximum applied indentation load, E is the
elasticity modulus, H is hardness, and c is the length of the
surface radial crack measured from the center of the indenta-
tion hole. α is an empirically determined calibration constant
which can be taken 0.04 for sharp indenters, such as
Berkovich [24].
To calculate the fracture toughness values of the samples,
the length of surface radial crack (c in equation (3) is measured
from the AFM images. Figure 7a–d illustrates the AFM im-
ages of the nano-indentation holes and the corresponding sur-
face radial cracks for the enamel under the bracket and the
intact enamel of both adhesive groups. Due to some variations
in the crack length, at least ten measurements of the crack
length were taken and the average value of crack lengths
was used in equation (3).
E and H in equation (3) are obtained from separate nano-
indentation tests in which no radial cracks were observed
around the indentation hole. Meanwhile, for investigating
the effect of bracket bonding-debonding on fracture toughness
of enamel, cracks should be created around the indentation
holes both at the intact and at the under-the-bracket enamel.
Through all the samples tested in this study, cracks were gen-
erated at both the under-the-bracket and the control regions

Fig. 3 A sample load-

displacement curve obtained from
the nano-indentation test and its
tangent line to the unloading
segment at the maximum load
Exp Mech
Fig. 4 Repeatability of load-
displacement curves obtained
from the nano-indentation test on
the under-bracket enamel for one
of the test specimens
only in four samples. In other samples, crack was generated
either in none of the two regions or only in one region. There-
fore, the fracture toughness results obtained in these two re-
gions could be compared only for those four samples.
Results
Figure 5 shows the elasticity modulus values of enamel under
the bracket and intact enamel.
The mean value of elasticity modulus discrepancy between
the two regions for the teeth in which brackets were bonded by
composite adhesive is equal to 17.06 GPa (with standard de-
viation of 6.20 GPa) and for those with brackets bonded by
nano-composite is equal to 54.64 GPa (with standard
Fig. 5 Elasticity modulus values in both regions for samples in which the brackets were bonded by a) composite adhesive and b) nano-composite
adhesive
deviation of 9.59 GPa). Comparison of these results shows
that the elasticity modulus discrepancy in the nano-
composite case is more than that of the composite adhesive
case. Using independent sample t-test demonstrates that the
differences between the two groups are statistically significant
(p-value<0.001).
Figure 6 shows the normal hardness values of enamel un-
der the bracket and intact enamel calculated according to the
above description for all samples.
The mean value of hardness differences between the
intact enamel and the enamel under the bracket for speci-
mens in which bracket bonded by composite adhesive is
equal to 0.64 GPa (with standard deviation of 0.21 GPa)
and for those in which bracket bonded by nano-composite
is equal to 1.60 GPa (with standard deviation of
 Exp Mech

Fig. 6 Normal hardness values of enamel under the bracket and intact enamel for samples of, a) composite group and b) nano-composite group

Fig. 7 The AFM images of nano-indentation hole and the surface radial crack around it for a) intact enamel of composite adhesive group, b) under-the-
bracket enamel of composite adhesive group, c) intact enamel of nano-composite group and d) under-the-bracket enamel of nano-composite group
Exp Mech
0.37 GPa). Using independent sample t-test indicates that
the differences between the two groups are statistically
significant (p-value<0001).
The values of fracture toughness (Kc) calculated by equa-
tion (3) for the intact enamel and enamel under the bracket are
presented in Table 1.
The difference between the fracture toughness values of the
intact enamel and under-the-bracket enamel was obtained for
each sample. The mean value of fracture toughness differ-
ences between the intact enamel and enamel under the bracket
for specimens in which bracket bonded by composite adhe-
sive is equal to 0.42 MPa.m1/2 (with standard deviation of
0.06 MPa.m1/2) and for those with bracket bonded by nano-
composite is equal to 0.54 MPa.m1/2 (with standard deviation
of 0.09 MPa.m1/2). Using independent sample t-test illustrates
that the difference between the effect of bracket bonding-
debonding on the fracture toughness of two groups isn’t sta-
tistically significant (p-value=0.07). This means that the use
of composite or nano-composite for bonding orthodontic
brackets have similar effects on the fracture toughness of the
enamel.
However, fracture toughness of the enamel decreases after
bonding and debonding the orthodontic brackets for all sam-
ples. The use of independent sample t-test demonstrates that
the difference between the fracture toughness values at the
intact enamel and under the bracket enamel for each group is
statistically significant (p-value<0.05).
Discussion
The results obtained in this study refuse our hypothesis that
bonding orthodontic brackets with the nano-composite adhe-
sive will reduce damage in the under-the-bracket enamel. As
illustrated in Fig. 5, the elasticity modulus of intact enamel is
more than that of enamel under the bracket, for all samples.
Thus, the elasticity modulus of enamel decreases after bracket
bonding and debonding for both composite and nano-
composite adhesives. However, this reduction is higher for
the cases where brackets were bonded by nono-composite.
The reduction in the elasticity modulus of enamel after bracket
bonding and debonding may be due to the increase in the
Table 1 The values of fracture toughness (Kc) in MPa.m1/2 for the intact enamel and the under-the-bracket enamel in both groups of dental adhesives
Composite adhesive group
Sample number Intact enamel Under-the-bracket enamel
1 0.86 0.36
2 1.05 0.63
3 0.80 0.45
4 1.06 0.65
enamel porosity caused by etching the enamel surface under
the bracket. Enamel etching dissolves Hydroxyapatite (HA)
crystals of the enamel surface [25, 26]. The results reported in
previous studies indicate that HA prismatic crystals are very
hard and the main reason for the dental enamel hardness and
stiffness is the regular and dense arrangement of these crystals
in the enamel microstructure [27, 28]. Therefore, dissolving
HA crystals of dental enamel under the bracket may cause a
decrease in the stiffness and consequently in the elasticity
modulus of enamel at this site.
The penetration of adhesives, which are used for orthodon-
tic bracket bonding, into the enamel porosities compensates
partially the reduction of enamel stiffness and elasticity mod-
ulus due to etching. As a potential reason, one may suggest
that the molecular bonds created between the penetrated ad-
hesive and the enamel molecules reduce the porosities of
enamel surface. Previous studies [11, 29] have shown that
the structure of nano-composite adhesives is more compact
than that of the composite adhesives. As a result, nano-
composites have higher viscosity than composite adhesives
and penetrate hardly into the enamel porosities caused by
etching. Therefore, the elasticity modulus reduction at enamel
under the bracket in nano-composite samples used is more
than that of composite samples.
Based on Fig. 6, the hardness values of all samples at the
intact enamel are more than the corresponding values at enam-
el under the bracket. This is in agreement with the study of
Lijima et.al. which used dental composite adhesives by differ-
ent etching systems for orthodontic bracket bonding [4].
Two factors might affect the reduction of hardness at enam-
el under the bracket:
1. The increase in the enamel porosity caused by etching the
enamel surface under the bracket.
As discussed previously, enamel etching dissolves the
HA crystals of its surface which increases the enamel
porosity and hence decreases hardness and elasticity mod-
ulus of enamel. However, the penetration of bracket bond-
ing’s adhesive in the enamel porosities fill up them rela-
tively. Meanwhile, previous researches have demonstrat-
ed that hardness of these adhesives is significantly less
than enamel hardness [30, 31]. Thus, enamel under the
Nano-composite group
Sample number Intact enamel Under-the-bracket enamel
1 0.72 0.32
2 0.95 0.37
3 0.86 0.28
4 0.85 0.26

bracket deforms more than intact enamel in the nano-
indentation test.
2. The creation of micro cracks on the enamel caused by
bracket debonding.
Bracket debonding creates micro cracks on the enamel
surface, as shown in previous studies [32, 33]. Thereby,
the deformation of enamel surface caused by immersing
the indenter is increased when the indent is made on a
cracked surface and causes the degradation of enamel
hardness.
The hardness reduction at the enamel under bracket in
specimens wherein bracket bonded by nano-composite is
more than the corresponding values of those with bracket
bonded by composite adhesive. As explained in previous
section, higher viscosity of the dental nano-composite in
comparison with the composite adhesive makes them
stiffer to penetrate into the enamel porosities. Therefore,
by using dental nano-composite more porosity remains in
the enamel of teeth, which causes higher reduction of
hardness at enamel under the bracket.
As shown in our recent study [10], less force is required for
debonding the brackets bonded by the nano-composite adhe-
sive compared to those bonded by the composite adhesive,
and a combination of cohesive and adhesive failure occurs at
the enamel-adhesive and the bracket-adhesive interfaces in
both groups. Thus, no reason exists for further enamel damage
in the nano-composite group. As a result, one may suggest
that the main reason for higher degrading effects of nano-
composite adhesive on the enamel hardness is the residual
enamel porosities as discussed in detail earlier.
The reduction in fracture toughness of the enamel after the
bonding-debonding of bracket may be due to the following
reasons:
1. As discussed earlier, dissolving the HA crystals caused by
enamel etching, increases the enamel porosity and hence
decreases the resistance of enamel against crack propaga-
tion. Moreover, local stress concentrations are increased
in the enamel surfaces having higher porosity.
2. Bracket debonding after (or during) the orthodontic treat-
ment causes some damages to the teeth enamel under the
bracket region. Despite recent advances in orthodontics
brackets, in bracket debonding methods and in debonding
instruments, the creation of damage in the teeth enamel
such as fractures and other surface defects during the
bracket debonding stage is still a serious concern in the
orthodontic treatments [4, 10]. Such damages in the
enamel surface deteriorate its surface properties including
fracture toughness.
It is worth mentioning that the scatter in the mechanical
properties obtained in this study from different teeth samples
Exp Mech
is due to the variety of the chemical and physical properties of
the teeth, which belong to different people.
Conclusions
Nano-indentation experiments were performed on enamel
section of human tooth to investigate the effect of bracket
bonding-debonding in samples where the brackets were bond-
ed by composite adhesive and by nano-composite one. It was
found that:
1. Elasticity modulus of enamel decreased after bracket
bonding-debonding for both composite and nano-
composite adhesives.
2. The reductions in the elasticity modulus and hardness of
enamel under the bracket were more in samples prepared
by nano-composite adhesive.
3. Hardness values of all samples at the intact enamel were
more than the corresponding values at enamel under the
bracket.
4. Fracture toughness of the enamel decreased after bonding
and debonding of the orthodontic brackets for all samples.
5. The use of composite and nano-composite adhesives for
bonding the orthodontic brackets on the teeth had almost
the same degrading effects on the fracture toughness of
enamel.
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