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Evaluation of shear bond strength of
primer-treated ceramic bracket on
dental zirconia surface
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Abstract
Evaluation of shear bond strength of
primer-treated ceramic bracket on
dental zirconia surface
Division of Dental Biomaterials Science
Department of Dental Science, Graduate School
Seoul National University
(Directed by Prof. Shin Hye Chung)
Ga Youn Ju
This study aims to evaluate the shear bond strength (SBS) of ceramic
primer-treated ceramic bracket on dental zirconia and to compare with
the SBS of ceramic bracket on conventionally treated dental zirconia.
Zirconia (LAVA Plus, 3M ESPE, St. Paul, MN, USA) samples were
sintered and polished with 500 grit diamond disc. The surface was
sandblasted with 50 μm alumina and treated as follows: no treatment of
the primer (X), treatment of the primer on the zirconia (Z), treatment of
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the primer on the bracket base (B), and treatment of the primer on both
the zirconia and the bracket base (ZB). The ceramic bracket (Perfect
Clear II, Hubit, Uiwang, Korea) was bonded on the zirconia surface with
the orthodontic resin. The SBS was measured before (T0) and after the
10,000 cycles of thermocycling (T10000). After the SBS test, the bond
failure interface was explored under FE-SEM and Adhesive Remnant
Index (ARI) was evaluated. Statistical significance of the data of SBS
was analyzed using the program (α = 0.05).
In T0 and T10000, significantly high SBS was obtained in ZB (primer
on both the zirconia and the bracket base) (p < 0.05). There was no
significant difference in SBS between Z (primer on the zirconia) and B
(primer on the bracket base). The adhesive failure occurred at zirconia-
resin interface in B while Z showed adhesive failure at resin-bracket
interface. In ZB, mixed failure was shown at the zirconia-resin-bracket
bonding interfaces.
The highest SBS was obtained when the ceramic primer was treated to
both the zirconia and the bracket base. The application of the ceramic
primer on the bracket base increased bonding strength to the level of the
ceramic primer treated zirconia.
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Keywords: dental zirconia, ceramic primer, ceramic bracket, shear bond
strength, surface treatment
Student Number: 2015-30620
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Contents
1. Introduction .................................................................................... 1
2. Materials and Methods .................................................................. 4
2.1. Specimen Preparation ...................................................................... 4
2.2. Surface Treatment and Bracket Bonding .......................................... 4
2.3. Microstructure Observations ............................................................ 5
2.4. Shear Bond Testing and Failure Mode Observations ........................ 8
3. Results .......................................................................................... 10
3.1. Microstructure Observations .......................................................... 10
3.2. Shear Bond Testing and Failure Mode Analysis ............................. 10
4. Discussion ..................................................................................... 20
5. Conclusion .................................................................................... 25
References ........................................................................................ 26
Abstract in Korean........................................................................... 30
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1. Introduction
Increasing interest in aesthetics and the need to overcome the
disadvantages of traditional porcelain fused metal crown, such as low
strength of porcelain and greyish shade of gingiva from metal
substructures, have led to the development of a wide range of ceramic
systems (1-3). Amongst them, the use of dental zirconia has increased
recently. Polycrystalline zirconia is a frequently used ceramic system in
load bearing area with aesthetic demands, primarily consists of yttria
stabilized tetragonal zirconia polycrystal (Y-TZP) (4-6). The phase
transformation of Y-TZP from tetragonal to monoclinic under stress
conditions increases the particle volume, which inhibits crack
propagation, resulting in high flexural strength (4, 5, 7). Due to high
mechanical properties, it has been used in inlays, onlays, crowns, post
and core systems, and as frameworks for porcelain fused zirconia (PFZ)
restorations (5, 6, 8, 9). Although PFZs provide enhanced aesthetics,
chipping and delamination of the veneered porcelain limit their use in
dental restoration (5, 6, 10). Together with the development of zirconia
with increased translucency, the use of full-contoured zirconia (FCZ) is
increasing for both anterior and posterior restorations (6).
The zirconia is acid-resistant because it does not contain silica
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particles while most dental ceramics contain that. This makes it less
responsive to hydrofluoric acid etching, which is an effective surface
treatment method for other glass ceramic systems (3, 6, 11-16). To
enhance the resin bond strength on zirconia, air particle abrasion or
tribochemical silica coating were suggested (11-13, 15). However, in the
latter case, the attachment of silica on the zirconia surface was not
predictable after the artificial aging processes (11). In case of the zirconia
restorations, application of primers or bonding systems with functional
monomers (eg, 10-methacryloyloxydecyl dihydrogen phosphate; 10-
MDP) on the roughened surface showed increased bonding strength (11,
15).
As the number of adult patients performing orthodontic treatment
is growing, the cases of bracket bonding on zirconia restorations are
increasing. A bracket bonding failure on posterior teeth can be solved by
using orthodontic metal bands, while in anteriors, bonding is more
challenging because of aesthetic considerations. Studies have conducted
on the bonding between feldspathic porcelain and brackets (17-19).
However, there are not many studies about FCZ and ceramic bracket
although it requires a different bonding protocol. A study reported that
silane treatment on glazed FCZ was sufficient to achieve adequate bond
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strength (20). Yet another study reported that sandblasting and 10-MDP
containing primer application on glazed zirconia surface was effective
(21). Still, bonding ceramic bracket on FCZ is controversial. It is
believed that there is a need for more studies about a protocol for
obtaining bonds that are time/cost-effective and have long-term stability.
This study aims to evaluate the shear bond strength of primer-
treated ceramic bracket on dental zirconia and to compare with
conventional zirconia surface treatment. The null hypotheses were; 1)
The primer application on zirconia does not enhance the bond strength;
2) The primer treatment on bracket base does not enhance the bond
strength.
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2. Materials and Methods
2.1. Specimen Preparation
Eighty zirconia (LAVA Plus, 3M ESPE, St. Paul, MN, USA)
specimens in 15 (width) × 15 (height) × 3 (thickness) mm were prepared
from a green stage zirconia block and the specimens were sintered by
following manufacturer’s instructions. Each specimen was embedded in
a polyester resin (EC-304, Aekyung, Seoul, Korea) and polished with a
diamond disc (MD-Piano, Struers, Ballerup, Denmark) up to 500 grit
under water irrigation. The surfaces of the all samples were sandblasted
with 50 �m alumina (SandStorm Expert, Vaniman, Fallbrook, CA, USA)
from a distance of 20 mm for 20 sec in a circular motion under a pressure
of 400 kPa. The samples were cleaned in an ultrasonic bath with distilled
water for 2 min and dried.
2.2. Surface treatment and Bracket Bonding
All the zirconia samples were randomly divided into 4 groups (n
= 20). All the zirconia surfaces were roughened by alumina sandblasting.
In X, no surface treatment was done on the alumina blasted zirconia
surface. In Z, a ceramic primer (CP; Clearfil ceramic primer, Kuraray,
Tokyo, Japan) was applied on the zirconia surface. In B, CP was applied
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on the bracket base. In ZB, CP was applied on both the zirconia surface
and the base of the bracket. After the surface primer treatment, the
adhesive primer (Transbond XT adhesive primer, 3M Unitek, Monrovia,
CA, USA) was applied on the zirconia surface and the bracket (Perfect
Clear II, Hubit, Uiwang, Korea) was bonded using the adhesive paste
(Transbond XT adhesive paste, 3M Unitek) under gentle pressure.
Excess resin was removed and light cured (Elipar Free Light 2, 3M ESPE,
St. Paul, MN, USA) for 10 sec on each side of the bracket for a total of
40 sec. A flow chart of experiment is shown in Figure 1. The composition
of the materials used in this study is shown in Table 1.
2.3. Microstructure Observations
The surface of the intact bracket base was observed under field
emission scanning electron microscopy (FE-SEM; S-4700, Hitachi,
Tokyo, Japan). The retentive structures of the intact bracket base were
analysed with an energy dispersive x-ray spectrometer (EDS; EMAX
7200H, HORIBA, England). Surface roughness (Ra) of the polished and
sandblasted zirconia surfaces was determined by using a confocal laser
scanning microscope (CLSM; LSM 800-MAT, Carl Zeiss MicroImaging
GmbH, Jena, Germany).
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Figure 1. Flowchart of the experiment. Ceramic primer (CP), control
group (X), group treated with CP on zirconia (Z), group treated with CP
on bracket (B), and group treated with CP on both the zirconia and the
bracket (ZB).
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Table 1. Materials used in this study
Materials Brand name LOT No. Composition Manufacturer
Zirconia LAVA Plus
515920
Tetragonal polycrystalline
zirconia, 3mol-% Yttria,
Alumina
3M ESPE,
USA
Primer
Clearfil
ceramic
primer
240010
3-Methacryloxypropyl
triethoxy silane, *10-MDP,
Ethanol
Kuraray,
Japan
Adhesive
Transbond
XT
adhesive
primer
ER7BS
Triethylene glycol
dimethacrylate,
Bisphenol A diglycidyl
ether dimethacrylate,
Triphenylantimony,
4-(Dimethylamino)-
Benzeneethanol,
dl-Camphorquinone,
Hydroquinone
3M Unitek,
USA
Composite
Resin
Transbond
XT
adhesive
paste
ER7BS
Silane treated quartz,
Bisphenol A diglycidyl
ether dimethacrylate,
Bisphenol A Bis(2-
hydroxyethyl ether)
dimethacrylate, Silane
treated silica
3M Unitek,
USA
*10-MDP (10-methacryloyloxydecyl dihydrogen phosphate)
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2.4. Shear Bond Testing and Failure Mode Observations
After the bracket bonding, the samples were stored in 100%
relative humidity at 37°C for 24 hour. The half of randomly distributed
samples were tested after 24 hour of storage. The other half underwent
aging process by a thermal circulator (DTRC-640, Jeiotech, Daejeon,
Korea) for 10,000 cycles at 5 ��and 55 ���The dwelling time was 30
sec and the transfer time was 20 sec. SBS was measured by using a
universal testing machine (Instron 8848, Instron, Norfolk County, MA,
USA) at a crosshead speed of 0.5 mm/min. The maximum load at failure
was calculated in MPa by dividing the maximum load (N) by the area of
the bracket base (12.24 mm2). The bond failure interface was evaluated
under FE-SEM and both failure mode and ARI was evaluated using
modified ARI scores (Table 2). Statistical analysis was performed by
Kruskal-Wallis test using the Statistical Package for the Social Sciences
(version 22.0; IBM Corp., Armonk, NY, USA) �������.
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Table 2. Criteria of modified adhesive remnant index (ARI) scores
1 Entire composite remained on the zirconia 2 More than 90% of the composite remained on the zirconia
3 More than 10% but less than 90% of the composite
remained on the zirconia
4 Less than 10% of the composite remained on the zirconia
5 No composite remained on the zirconia
Criteria Score
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3. Results
3.1. Microstructure Observations
The surface polished to with a diamond disc showed shallow
scratch lines without directionalities and average surface roughness (Ra)
of 0.10 �m. Sandblasted surfaces showed multiple short but deeper
scratches that were uniformly distributed and increased surface
roughness (Ra) to �����m (Figure 2). The bracket base showed multiple
spherical-shaped retentive beads (diameter of approximately 80 to 100
�m) attached to the surface except for the outer margin (approximately
� �m in width). The spherical shaped retentive beads showed
characteristic micro-rough surfaces and the EDS evaluation revealed that
they were mainly composed of aluminium (Figure 3).
3.2. Shear Bond Testing and Failure Mode Analysis
Before the thermocycling (T0), a significantly higher bonding
strength was obtained in ZB. Z and B had no significant difference. After
the thermocycling (T10000), reduced SBS was obtained when compared
with T0. The SBS was significantly decreased in X, B, and ZB in T10000
and was not significantly decreased in Z. Still, ZB, in which both the
zirconia and the bracket base were treated with ceramic primer, showed
highest SBS than the other groups in T10000 (Table 3, 4, 5, Figure 4).
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Figure 2. CLSM images of the zirconia surface before (A, C) (Ra: 0.10
�m) and after the sandblasting (B, D) (Ra�������m). Sandblasted surface
(B, D) showed evenly distributed micro-roughness.
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Figure 3. SEM images of the bracket base at ×30 (A) and ×300 (B). EDS
analysis of the spherical retentive microstructures (white diamond in B)
(C).
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Table 3. Comparison of SBSs (MPa) of the experimental groups
Group SBS (MPa, mean ± SD)
P value T0 (n = 10) T10000 (n = 10)
X 5.71 ± 0.48 Aa 2.03 ± 0.78 Db p = 0.000
Z 9.79 ± 1.94 Bc 8.16 ± 1.78 Ec p > 0.05
B 11.76 ± 2.55 Bd 8.49 ± 2.29 Ee p = 0.007
ZB 15.96 ± 2.49 Cf 11.65 ± 3.95 Fg p = 0.001
Same uppercase letters indicate no significant difference in each column and same
lowercase letters indicate no significant difference in each row.
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Table 4. P value between experimental group in T0 (p < 0.05)
T0 X Z B ZB
X - 0.000 0.000 0.000
Z - 0.249 0.000
B - 0.008
ZB -
Table 5. P value between experimental group in T10000 (p < 0.05)
T10000 X Z B ZB
X - 0.000 0.000 0.000
Z - 0.978 0.001
B - 0.003
ZB -
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Figure 4. Comparison of SBSs before (T0) and after (T10000) the
thermocycing (n = 10). Same uppercase letters indicate no significant
difference in T0 and T10000. Same lowercase letters indicate no
significant difference between T0 and T10000.
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A modified ARI score was used in the bonding failure measurements (22).
The criteria for modified ARI is shown in Table 2. Small amounts of
tagged resin left between the retention beads of the bracket were not
considered while scoring. In T0, all of the samples of X showed adhesive
failure at the zirconia and resin interface in which no resin was left on
the zirconia surface (ARI score 5). All of the samples of Z showed
adhesive failure at the resin and bracket interface in which all resin was
left on the zirconia surface (ARI score 1). Almost all the samples in B
showed adhesive failure at the zirconia and resin interface in which no
resin was left on the zirconia surface (ARI score 5). All the samples in
ZB showed mixed failure in which some resin was left on the zirconia
surface as well as on the bracket base (ARI score 3). In T10000, 90% of
the samples of X showed adhesive failure at the zirconia and resin
interface (ARI score 5). In Z, all showed adhesive failure at the resin and
bracket interface in which remnants of resin were left on all zirconia
surfaces regardless of thermocycling (ARI score 1). In B, adhesive
failures with no resin remained on the zirconia surface were mainly
occurred (ARI score 5). Almost all the samples in ZB showed mixed
failure in which some resin was left on the zirconia surface as well as on
the bracket base (ARI score 3) (Figures 5, 6, 7).
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Figure 5. Comparison of modified adhesive remnant index (ARI) scores
before (T0) and after (T10000) the thermocycling (n = 10).
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Figure 6. Representative SEM images of bonding failure observation of
T0 (×30). A and E showed adhesive failure at the zirconia-resin interface;
C showed adhesive failure at the resin-bracket interface; G showed
mixed failure at the zirconia-resin-bracket interface. Triangle (resin);
Square (captured resin between the retention beads).
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Figure 7. Representative SEM images of bonding failure observation of
T10000 (×30). A and E showed adhesive failure at the zirconia-resin
interface; C showed adhesive failure at the resin-bracket interface; G
showed mixed failure at the zirconia-resin-bracket interface. Triangle
(resin); Square (captured resin between the retention beads).
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4. Discussion
This study evaluated the effect of the MDP-containing ceramic
primer on the SBS of zirconia and the bracket. All the zirconia surfaces
were first uniformly grinded by 500-grit diamond disc to reproduce the
surface roughness of full-contoured zirconia crown made from a
diamond cutting bur. Then, the surfaces were sandblasted to increase the
surface area as used in bonding zirconia restorations. There is a concern
that the mechanical properties of zirconia are weakened by air-abrasion.
Still, micro-mechanical retention formed by sandblasting is preferred
since the bonding strength decreases dramatically when air-abrasion is
not performed (23, 24). The sandblasting conditions such as time,
particle size, pressure, and distance were set in this study to attain the
maximum bonding strength within a range in which the physical
properties of zirconia are not diminished (25).
The undercut and roughness of zirconia surfaces were increased
by sandblasting, but the results were limited due to hardness of zirconia.
Furthermore, decreased bonding strength was reported after the thermal
aging process (26). In control group X, which used Transbond XT
adhesion system after sandblasting without the primer treatment had the
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lowest SBS (5.71 MPa) compared with other groups in T0 and SBS
significantly decreased in T10000 (2.03 MPa). Without the primer
treatment, the bonding strength of 6–8 MPa required by natural teeth was
not achieved, and it can be assumed that it will have insufficient bonding
strength in clinical situations (27, 28).
It is known that chemical bonds in the zirconia and the primer are
achieved between the functional monomers of the primer and the metal
ions of the ceramic surface (29, 30). Treating the zirconia surface with a
functional monomer such as 10-MDP (10-methacryloyloxydecyl
dihydrogen phosphate) is recommended for improving the bonding
strength with resin (29-31). More specifically, direct bonding occurs
between the dihydrogen phosphate group of 10-MDP and the zirconium
ion of the zirconia surface; secondary van der Waals bonding or
hydrogen bonding also occurs. In addition, the bonding strength is
improved by enhancing the surface wettability of the zirconia ceramic
(32, 33).
A commercial MDP-containing primer was used to condition the
zirconia and bracket surfaces. In the previous studies, to obtain a long-
term bonding strength between zirconia and resin, 10-MDP primer in
combination with sandblasting of the zirconia surface was effective (33,
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34). The results of this experiment agree with this. When 10-MDP primer
was applied to zirconia (Z) or the base of the bracket (B), the SBS was
significantly higher. In case of T0, primer-treated group (Z, B and ZB)
had higher SBS than the control (X). A significantly higher SBS value
was observed when 10-MDP primer was applied to both the zirconia and
bracket surfaces (ZB). In case of T10000, the SBS in ZB was
significantly higher than in other experimental groups. It seemed that the
10-MDP containing primer clearly plays a role in increasing the bonding
strength between zirconia and resin and between the bracket and resin,
and the bonding strength differs according to the treated surface. Based
on the results, hypotheses 1 and 2 of this experiment were dismissed.
From the EDS analysis, a major component of the spherical
retentive bead on the surface of the bracket base was aluminium and
oxygen. Alumina also forms a chemical bond with the 10-MDP primer
because it is a metal oxide like zirconia (29). In B, on the primer-treated
bracket base, the possibility of chemical bond occurred between the
bracket and the primer is assumed to be contributed to the increased SBS.
Thermocycling is an artificial aging method to simulate the long-
term use of the brackets within the oral condition (35, 36). It can also
evaluate the hydrolysis resistance of the bonding interface (37).
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Performing 10,000 cycles of thermocycling has a similar effect as
approximately 12 months of their use in the mouth (38). Therefore,
considering the period of orthodontic treatment, this experiment
performed 10,000 cycles of thermocycling. Many previous studies have
reported that the SBS was greatly reduced after the thermocycling (39,
40). In the results of this study as well, the average SBS was reduced
after the thermocycling. However, Z, B, and ZB, which had primer-
treated surface, showed higher bonding strength than 6-8 MPa required
by natural teeth and brackets, even after the thermocycling. Therefore,
regardless of which surface is treated, the clinically required level of
bracket bonding strength is available on the zirconia through surface
treatment using ceramic primer.
In case of T0 and T10000, about ARI, results that the resin had
continuity with the zirconia surface was shown in 100% of the samples
in Z. In 80-90% of the samples in B, there was no resin left on the
zirconia surface, and there was no significant difference between the
SBSs of group Z and group B. When the bracket is bonded to the zirconia
surface in dental clinics, the SBS can be raised if the primer is applied to
only the bracket base. The advantage of the ceramic bracket priming is
the preservation of the surface of restorations. When dealing with
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orthodontic brackets, removing should be concerned after the certain
period. If the surface treatment is only limited on the restoration, the
higher the bond strength, the higher the possibility of the surface fracture.
The increased bond strength in the primer treated bracket, supported by
the results from ARI, it also gives the benefit of obtaining a better
zirconia surface integrity when the bracket is removed.
When the primer was applied to the adhesion surface of the
ceramic bracket (B), without surface treatment of the zirconia surface,
the bonding strength was increased to the level of zirconia surface
treatment (Z). In SBS testing, the bonding failure occurs at the point
where the load is concentrated. After the primer application on the
bracket surface, it is considered that the stress distribution becomes
uniform by acting as a single unit composed of ceramic and resin
resulting in the increased SBS. Further study, using techniques such as
finite element analysis to examine the reason is needed to explain the
increase in the SBS despite the occurrence of adhesive failure between
the zirconia and the resin when the primer is applied to the bracket base.
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5. Conclusion
The following conclusions were obtained by this study; The primer
application on bracket base enhanced bonding strength as well as the
ceramic primer on zirconia; Applying the ceramic primer to both the
zirconia and the bracket base showed highest bonding strength. In
clinical practice, when sufficient bonding strength is required between
ceramic bracket and zirconia, ceramic primer application on both surface
is recommended.
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1. Introduction2. Materials and Methods2.1. Specimen Preparation2.2. Surface Treatment and Bracket Bonding2.3. Microstructure Observations2.4. Shear Bond Testing and Failure Mode Observations
3. Results3.1. Microstructure Observations3.2. Shear Bond Testing and Failure Mode Analysis
4. Discussion5. ConclusionReferencesAbstract in Korean
81. Introduction 12. Materials and Methods 4 2.1. Specimen Preparation 4 2.2. Surface Treatment and Bracket Bonding 4 2.3. Microstructure Observations 5 2.4. Shear Bond Testing and Failure Mode Observations 83. Results 10 3.1. Microstructure Observations 10 3.2. Shear Bond Testing and Failure Mode Analysis 104. Discussion 205. Conclusion 25References 26Abstract in Korean 30