Evaluation of Microshear Bond Strength of Orthodontic

Resin Cement to Monolithic Zirconium Oxide as a

Function of Surface Conditioning Method
Nehir Canigur Bavbeka / Jean-Franois Rouletb / Mutlu zcanc

Purpose: To evaluate the microshear bond strength (SBS) of orthodontic resin cement to monolithic zirconium
oxide ceramic (MZ) after different surface conditioning methods.
Materials and Methods: Two types of MZ (BruxZir Solid Zirconia, n = 60; Prettau-Zirkon, n = 60) with two types
of surface finish (glazed, n = 30 per group; polished, n = 30 per group) were tested after two surface conditioning methods: 1. air abrasion with 30-m silica coated aluminum oxide (Al2O3) particles (CoJet), or 2. air abrasion
with 50-m Al2O3 particles. The non-conditioned group acted as the control. A universal primer (Monobond-Plus)
and an orthodontic primer (Transbond-XT Primer) were applied to all specimen surfaces. Orthodontic resin composite (Transbond-XT) was bonded using a mold and photopolymerized. The bonded specimens were subjected
to SBS testing (0.5 mm/min). Data were analyzed statistically using three-way ANOVA and the Sidac adjustment post-hoc test ( = 0.05). Failure modes were analyzed using a stereomicroscope (30X).
Results: Mean SBS values (MPa) did not show a significant difference between the two brands of MZ
(p > 0.05). In both glazed (44 6.4) and polished (45.9 4.8) groups, CoJet application showed the highest SBS values (p < 0.001). The control group (34.4 6) presented significantly better results compared to
that of Al2O3 (30 3.8) (p < 0.05) on glazed surfaces, but it was the opposite in the polished groups (control:
20.3 4.7; Al2O3: 33.8 4.7; p < 0.001). Adhesive failure was the dominant type in all groups. Conditioning
MZs with Al2O3 and CoJet increased the percentage of mixed failure type.
Conclusion: Air abrasion with CoJet followed by the application of universal primer improved the SBS of orthodontic resin to both the polished and glazed monolithic zirconium oxide materials tested.
Key words: air abrasion, monolithic zirconium oxide, zirconia, microshear bond strength, orthodontic bonding,
surface conditioning method.
J Adhes Dent 2014; 16: 8 pages
doi: 10.3290/j.jad.a32812

oday, technological developments in dental materials

allow clinicians to offer oral rehabilitations with more
esthetic outcomes using fixed dental prostheses (FDP)

Research Assistant, Department of Orthodontics, Faculty of Dentistry, Gazi

University, Ankara, Turkey. Idea, prepared the specimens, performed the
experiments, wrote the manuscript, discussed the results and commented
on the manuscript at all stages.

Professor, Department of Restorative Dental Sciences, College of Dentistry,

University of Florida, Gainesville, FL, USA. Contributed to the hypothesis,
experimental design, monitored specimen preparation and experiments,
proofread the manuscript, discussed the results and commented on the
manuscript at all stages.

Professor, Clinic for Fixed and Removable Prosthodontics and Dental Materials
Science, Center for Dental and Oral Medicine, Dental Materials Unit, University of Zrich, Zrich, Switzerland. Contributed to the experimental design,
consulted on statistical evaluation, contributed to writing the manuscript, discussed the results and commented on the manuscript at all stages.

Correspondence: Nehir Canigur Bavbek, Gazi University, Faculty of Dentistry,

Department of Orthodontics, 8. Cadde, 82. Sokak, 06510 Emek, Ankara, Turkey.
Tel: +90-505-4282674; Fax: +90-312-2239226. e-mail: ncanigur@yahoo.com

doi: 10.3290/j.jad.a32812

Submitted for publication: 22.01.14; accepted for publication: 12.08.14

without compromising strength and durability. Due to

the increased esthetic demands of the patients, porcelain-fused-to-metal (PFM) FDPs are often replaced with
all-ceramic FDPs5 that are optically appealing, biocompatible, color stable, and resistant to wear.40 Despite
these advantages, their brittle nature has restricted
their use.44
The efforts to develop a new FDP material with a strong
framework similar to PFM FDPs but at the same time being as esthetic as glassy-matrix ceramics resulted in the
introduction of zirconium oxide. In particular, 2 to 3% mol
yttria (Y2O3) containing the tetragonal zirconia polycrystalline (Y-TZP) form of zirconium oxide has become prevalent.
Currently, this material is widely used for frameworks of
all-ceramic FDPs due to its biocompatibility, high flexural
strength, wear resistance, and fracture toughness.11,24,39
Previous studies reported service-life expectations of Y-TZP
zirconium oxide core that were comparable to PFM FDPs for
posterior indications.16,39,40 However, after routine clinical
use, reported disadvantages such as chipping or delamina1

Canigur Bavbek et al

tion of veneering ceramic5,16 posed a clinical challenge. In

order to overcome this problem, monolithic zirconium oxide
(MZ) was introduced on the dental market.
Fabrication of FDPs from MZ is a new technology which
is expected to gain substantial interest as it provides high
strength, esthetics, and easy fabrication at lower costs.19
Full-contour MZ FDPs are milled from blocks using CAD/
CAM technologies and can be used either polished or
glazed for improved optical results.38 Although polishing decreases the surface roughness and may provide sufficient
esthetics, many MZ FDPs are glazed superficially during
laboratory procedures to improve their optical properties.
In addition, glass particles infiltrated into zirconium oxide
surfaces such as in glazing could enhance the adhesive
bonding, as it can be etched and silanized with silane
coupling agents.49
Despite its advantages, the chemical or mechanical
bond between the adhesive resins and oxide ceramics is
still inferior to that between adhesive resins and glassy
matrix ceramics.2,41 Unlike porcelain surfaces, oxide ceramics are not etchable and their glass-free nature reduces favorable silane reaction.2,5,20 Alternative conditioning methods have been discussed in the literature for
resin bonding to zirconium oxide. Some authors reported
that roughening the surface for mechanical interlocking
and using a composite resin containing phosphate monomer showed promising in vitro bond strength values45 and
clinical survival rates.36 Others proposed tribochemically
silica coating the surface with silica-coated alumina particles, followed by silane application for effective bonding.2,26 However, relying on aggressive abrasion methods
for successful mechanical bonding may initiate surface
flaws in the material and diminish its strength.47,48
The increased awareness of adult patients of dental
esthetics has resulted in more adults seeking orthodontic
treatment.21 Consequently, orthodontists started facing
substrates other than enamel onto which orthodontic appliances must be bonded.32 Potentially, a lack of bonding protocols in orthodontics for such new materials may
yield early debonding of fixed appliances. To date, several
studies have addressed different surface conditioning protocols for orthodontic bonding to porcelain materials that
are widely used for fabrication of FDPs. These approaches
vary from mechanical roughening of the surface using airborne particle abrasion,14,22,35 tribochemical silica coating,35 chemical conditioning with hydrofluoric acid etching
or application of silane coupling agents,8,20 or a combination of both mechanical and chemical methods.4,35,42
However, to the authors best knowledge, no information
is available on how to bond onto MZ for orthodontic procedures. Considering the popularity and increasing demand for MZ crowns in general dental practice, bonding
brackets to this material in its polished or glazed form
necessitates the development of a protocol for bonding
procedures for orthodontic applications.
The objectives of this study therefore were to evaluate the effects of different surface conditioning methods
on the microshear bond strength of an orthodontic resin
composite to polished or glazed MZ materials and to analyze the failure types after debonding. The following null
2

hypotheses were tested: 1) Surface conditioning methods would not improve adhesion compared to the control
group, 2) adhesion on polished or glazed MZ would not
differ, 3) adhesion to high purity MZ would not differ from
that to yttria-stabilized MZ.

MATERIALS AND METHODS

The types, brands, manufacturers, chemical compositions, and batch numbers of the materials used in this
study are listed in Table 1.
Specimen Preparation
Two different monolithic zirconium oxide (MZ) materials
were tested in this study, MZ1 (BruxZir Solid Zirconia,
Glidewell Dental Laboratories; Newport Beach, CA, USA)
and MZ2 (Prettau-Zirkon, Zirkonzahn; Neuler, Germany).
While MZ1 specimens were obtained from the manufacturer already sintered and polished (5 mm 5 mm),
MZ2 specimens were received in nonsintered in blocks.
They were cut into squares (6 mm 6 mm) approximately
20% greater than the size of sintered MZ1 specimens in
order to compensate for the sintering shrinkage. They
were then sintered in a furnace at 1500C (Sintramat
High Temperature Furnace, Ivoclar Vivadent; Buffalo, NY,
USA) with a heating rate of 8C/min and a holding time of
two hours. After sintering, they were polished with rubber
disks (Shofu Dental; San Marcos, CA, USA).
Square-shaped (5 mm 5 mm) MZ1 and MZ2
specimens were polished under water using 600-, 800and 1200-grit silicon carbide abrasive papers in sequence
and ultrasonically cleaned in distilled water for 1min.
Specimens (N = 120, n = 60 per brand) from each MZ
brand were randomly divided into two subgroups. Half
of the specimens were polished and the other half were
glazed. The first group of specimens from each product (n = 30) was left as polished, whereas the second
group (n = 30) was glazed (Gl) after polishing. Glazing
was performed using a spray glaze (Prismatik Universal
Low Fusing Spray Glaze, Glidewell Direct; Irvine CA, USA)
according to the manufacturers recommendations. The
specimens were then fired in a furnace at 870C for 90 s
holding time without vacuum (Jelrus International Wizard
Dental Porcelain Oven Furnace, Jelrus; Melville, NY, USA).
All specimens were then embedded in autopolymerizing acrylic resin (powder and liquid, Acratray Blue, Henry
Schein; Melville NY, USA) with their glazed and polished
surfaces exposed. First, the specimens were held in place
on a smooth surface with a piece of two-sided adhesive
tape. Then, powder and liquid of acrylic resin was mixed
(1:3) and poured into the molds to produce cylinders measuring 2.54 cm in diameter and 2.54 cm in length (Ultradent
Products; South Jordan, UT, USA). After auto-polymerization
started, the mold was placed in a container in cold water to
decrease the polymerization temperature. After polymerization, the cylinders were removed from the mold and the twosided adhesive tape was removed. The specimen surfaces
were then cleaned with ethanol. The acrylic bottom of the
cylinders was ground with 120-grit silicon carbide abrasive
The Journal of Adhesive Dentistry

Canigur Bavbek et al

Table 1 Types, brands, manufacturers, chemical compositions, and batch numbers of the materials used in this study
Type and brand

Manufacturer

Chemical composition

Batch number

BruxZir Solid Zirconia

Glidewell Dental Laboratories;

Newport Beach, CA, USA

High purity ZrO2

NA*

Prettau-Zirkon

Zirkonzahn; Neuler, Germany

ZrO2 (70-97%), Y2O3 (<6%), HfO2 (<5%), Al2O3 (<1%), SiO2

(max 0.02%), Fe2O3 (max 0.01%), Na2O (max 0.04%)

ZB2195A

Prismatik Universal
Low Fusing Spray Glaze

Glidewell Direct; Irvine CA,

USA

Sodium, potassium, boron and aluminum silicate glass

(11-21%), isopropyl alcohol (17-27%), isobutane (51-61%)

11413

Acratray Acrylic Powder

(Blue)

Henry Schein; Melville NY,

USA

Particulates, calcium carbonate, titanium dioxide, benzoyl peroxide

140513

Acrylic Liquid (Self cure)

Henry Schein

Methyl methacrylate, benzophenone, hydroquinone

700313

CoJet Sand

3M ESPE; St Paul, MN, USA

30-m SiOx

506649

Pure Blast Al2O3 Sand

Henry Schein

50-m Al2O3 particles

572703

Monobond Plus

Ivoclar Vivadent; Schaan,

Liechtenstein

Ethanol, 3-trimethoxysilylpropyl methacrylate, methacrylated phosphoric acid ester, disulfide methacrylate

R85603

Transbond XT Primer

3M Unitek; Monrovia, CA, USA

Bisphenol-a diglycidyl ether dimethacrylate (bis-GMA),

triethylene glycol dimethacrylate, 4-(dimethylamino)-benzeneethanol, dl-camphorquinone, hydroquinone

N480229

Transbond XT Light Cure

Orthodontic Adhesive

3M Unitek

Silane-treated quartz, silane-treated silica, bisphenol-a

diglycidyl ether dimethacrylate (bis-GMA), bisphenol A
BIS (2-hydroxyethyl ether) dimethacrylate, diphenyliodonium hexafluorophosphate

N495216

*Provided by the manufacturer.

Experimental Sequence

Zirconium Oxide Material

MZ1
Polished
Control

AL2O3

Surface Finish

Glazed
CoJet

Control

AL2O3

MZ2

CoJet

Surface Conditioning

Polished
Control

AL2O3

Glazed
CoJet

Control

AL2O3

CoJet

Universal Primer Application (Monobond Plus)

Adhesive Resin Application (Transbond XT Primer)

Orthodontic Resin Composite Application (Transbond XT Adhesive)

Fig 1 Experimental groups and conditioning sequences of zirconium oxide materials. MZ1: BruxZir Solid Zirconia; MZ2: PrettauZirkon.

paper under running water for about 1min to ensure that

they were parallel to the bottom surface of the clamp into
which the cylinders were placed during bonding.
The polished and glazed MZ1 and MZ2 specimens were
further randomly divided into three subgroups according to
the surface conditioning method (n = 10 per group) (Fig 1).
doi: 10.3290/j.jad.a32812

Surface Conditioning Methods

The nonconditioned group served as control.
Air abrasion with Al2O3: Specimen surfaces were air
abraded with an intraoral air-abrasion device (Microetcher,
Danville Engineering; San Ramon, CA, USA) with 50-m
Al2O3 powder (Pureblast White no. 100-3954, Henry
3

Canigur Bavbek et al

Fig 2 Specimen preparation and microshear bond testing: a)

upper view of fixing substrate to a clamp to achieve flat substrate surfaces; b) side view of substrate fixation; c) debonding
the resin composite from zirconium oxide surface using a special loading jig (Ultradent Products).

Schein; Melville NY, USA) perpendicular to the surface

from a distance of approximately 10 mm for 20 s in circling motions at 2.8bar. After air abrasion, the specimen
surfaces were gently air blown to remove the remnants of
the powder.
Air abrasion with silica-coated Al2O3: In this group,
specimen surfaces were air abraded with the same intraoral air-abrasion device as described for Al2O3 abrasion. This time, instead of 50-m Al2O3, 30-m silicacoated (SiOx) alumina particles were used (CoJet Sand,
3M ESPE; St Paul, MN, USA).
Bonding Procedures
Specimen surfaces were coated with a thin layer of
Universal Primer (Monobond Plus, Ivoclar Vivadent;
Schaan, Liechtenstein) that was left for 60 s to allow
it to react, and then gently air dried to evaporate the
solvent. Then, one coat of orthodontic adhesive primer
(Transbond XT Primer, 3M Unitek; Monrovia, CA, USA)
was applied with a microbrush, gently air dried, and
photopolymerized for 4 s using a photopolymerization
unit (1400 mW/cm2) (Valo Cordless LED Curing Light,
Ultradent Products). Each specimen was fixed to a
bonding clamp with a special mold (Ultradent Products)
to assure flat substrate surfaces and also to standardize the diameter (2.32 mm) of the resin composite
(Figs 2a to 2c). Orthodontic resin (Transbond XT Light
Cure Orthodontic Adhesive, 3M Unitek) was applied to
the surface using the bonding mold. Composite was
condensed in the mold and photopolymerized for 12s
(1400mW/cm2). The specimens were left for 24 h in a
dry environment at room temperature prior to testing.
Microshear Bond Strength (SBS) Test and Failure
Analysis
SBS testing was performed according to the Ultradent
testing method.18 The specimens were mounted to a test
base clamp (Ultradent Products) with the surfaces to be
4

tested facing the loading jig (Ultradent Products) fitted

to the universal testing machine (Instron Model 1125,
Instron; Norwood, MA, USA). The semicircular geometry of
the edge of the crosshead assembly facing the resin composite was specially designed to fit the tested resin from
the upper side, so that the force could be transferred
linearly and directly to the resin/substrate interface.
Maximum load (N) was applied at a crosshead speed of
0.5 mm/min and analyzed using Bluehill2 software for
Instron mechanical testing (Instron). The SBS values
were then calculated by dividing maximum load (N) by the
bonded area (4.227 mm2) of the tested composite.
After testing, the debonded surfaces of all specimens
were examined under a stereomicroscope (Stereomaster
Microscope, Fisher Scientific; Waltham, MA, USA) at 30X
magnification to identify the failure modes. Failure modes
were categorized as a) adhesive: failure between resin
composite and MZ, no composite resin remnants left on
MZ surface; b) cohesive: failure within the resin composite with a complete layer of resin left on MZ surface; or
c) mixed: surface had both adhesive and cohesive failure
characteristics, remnants of composite resin were left on
MZ surface, but the layer was not continuous.
Statistical Analysis
The power of the study was higher than 99% at = 0.05
with 10 specimens per group. Microshear bond strength
data (MPa) were submitted to three-way ANOVA with the
bond strength as the dependent variable and MZ materials (2 levels: BruxZir Solid Zirconia, Prettau-Zirkon),
surface finish (2 levels: polished, glazed), and surface
conditioning methods (3 levels: control, Al2O3 air abrasion, silica coating) as independent variables. Multiple
comparisons were made using the Sidac post-hoc test
( = 0.05). Statistical analysis was performed using
SPSS 15.0 software for Windows (SPSS; Chicago, IL,
USA). P-values less than 0.05 were considered to be
statistically significant in all tests.

RESULTS
While MZ type did not significantly affect the SBS (MPa)
of orthodontic resin composite (p = 0.74), surface finish
type (p = 0.003) and surface conditioning (p = 0.000)
had a significant influence (three-way ANOVA) (Table 2,
Fig 3). Interaction terms were significant only for air abrasion and surface finish methods (p = 0.000). The data of
MZ1 and MZ2 were pooled for further analysis of the effects of surface finish and surface conditioning.
Effect of Surface Finish
Air abrasion with Al 2O 3 generated higher SBS values on polished surfaces (33.8 4.7) than on glazed
ones (30 3.8) (p < 0.05) (Table 3). In contrast,
no surface treatment (control) performed better on
glazed (34.4 6) than polished surfaces (20.3 4.7)
(p < 0.001). There was no impact of surface finish on
mean SBS values for CoJet surface conditioning (polished: 45.9 4.8; glazed: 44 6.4) (p > 0.05).
The Journal of Adhesive Dentistry

Canigur Bavbek et al

Table 2 Three-way ANOVA of mean SBS values of orthodontic resin composite adhesion to monolithic zirconium
oxide as a function of surface finish and surface conditioning methods
Source of variation

Sum of squares

Degree of
freedom

Mean
square

F ratio

Significance

2.88

2.880

0.111

0.740

233.942

233.942

9.009

0.003

6670.986

3335.493

128.444

0.000

2.614

2.614

0.101

0.752

Material type surface conditioning

52.500

26.250

1.011

0.367

Surface finish surface conditioning

1923.491

961.745

37.035

0.000

Material type surface finish surface conditioning

130.294

65.147

2.509

0.086

2804.593

108

25.968

11821.298

119

Zirconium oxide material type

Surface finish
Surface conditioning
Material type surface finish

Error
Corrected total

Table 3
groups

SBS (MPa) results for the experimental

Table 4 Distribution of the frequencies of failure

types for experimental groups
Type of failure*

Surface finish
Surface
conditioning

Polished

Glazed

(Mean SD)

(Mean SD)

Control

20.3 4.7e,F

34.4 6c,C

<0.000

Al2O3

33.8 4.7d,D

30 3.8a,A

<0.05

CoJet

45.9 4.8b,E

44 6.4b,B

N.S.

<0.000

<0.05A,C;
<0.000A,B; B,C

MZ1

MZ2

ADHES COHES MIX

ADHES COHES MIX

p
Polished
Control
Al2O3
CoJet

10
6
4

0
0
0

0
4
6

10
7
4

0
0
0

0
3
6

10
5
5

0
0
0

0
5
5

8
7
9

0
0
0

2
3
1

Glazed
Control
Al2O3
CoJet

*Same lowercase superscript letters in each row, and same uppercase

letters in each column indicates no significant difference (Sidac post-hoc
test, = 0.05).

*ADHES: adhesive failure between resin composite and MZ, no composite resin remnants left on MZ surface; COHES: cohesive failure within
the resin composite with a complete layer of resin was left on MZ surface, MIX: surface had both adhesive and cohesive failure characteristics; remnants of composite resin were left on MZ surface, but the layer
was not continuous. MZ1: BruxZir Solid Zirconia; MZ2: Prettau-Zirkon.

Surface Finish and Surface Conditioning Interaction

For glazed MZ surfaces, mean SBS values of orthodontic composite were significantly higher with CoJet
application (44 6.4) than with Al 2 O 3 air abrasion
(30 3.8) (p < 0.001) and the control group (34.4 6)
(p < 0.001), but the control group showed significantly
higher results than the Al2O3 group (p < 0.05).
For polished MZ surfaces, mean SBS values were significantly higher with CoJet (45.9 4.8) than with Al2O3 air
abrasion (33.8 4.7) (p < 0.001) and the control group
(20.3 4.7) (p < 0.001). Further, the Al2O3 group showed
significantly higher SBS values than that of the control
group (p < 0.001).

Failure Mode
Examinations of the debonded specimens revealed failures predominantly at the MZ/resin composite interface
(adhesive), followed by the mixed failure type (Table 4).
No failure within the composite resin (cohesive) was observed. Air abrasion either with Al2O3 or CoJet increased
the frequency of mixed failures.

doi: 10.3290/j.jad.a32812

DISCUSSION
This study was undertaken in order to propose the best
bonding protocol for orthodontic resin cement to MZ
ceramics in their polished or glazed state. Based on the
5

Canigur Bavbek et al
60

Control
Al2O3
CoJet

40

45.9

20.3

33.8

44

MZ2
Polished

34.4

MZ2
Glazed

30

21.9
32.3
45.9

45.9

35.4

32.7
29.6
45.2

10

18.8

20

36.1

30
30.5
42.8

SBS (MPa)

50

0
MZ1
Glazed

MZ1
Polished

All
Glazed

results of this study, the first and second hypotheses

were rejected, as surface finish and surface conditioning methods significantly affected the results. Since the
two MZ brands did not show a significant difference, the
third hypothesis was accepted.
Most MZ FDPs are glazed or stained to improve the
esthetic results, but they can also be merely polished.
However, orthodontists may not be aware of the surface
characteristics of an MZ restoration to which they are
bonding, which is of clinical importance. For this reason,
both polished and glazed MZ were studied to decide on
a common bonding protocol for both surface finishes.
The results showed that regardless of the surface finish,
higher bond strength values were achieved with the CoJet application followed by the application of a universal
primer.
Bracket bond failure is one of the most common clinical problems in fixed orthodontic therapy. There are two
major interfaces that can be subject to debonding: the
enamel or restorative material/adhesive interface and the
adhesive/bracket interface. In this study, the microshear
bond strength test was performed for an orthodontic resin
composite, but the adhesive/bracket interface was not
evaluated. The reason for this was to eliminate possible
confounding factors such as geometry, mesh design of
the bracket base, or bracket material, all of which may
influence the test results.17,25 Isolating the interfaces
possibly involved in bracket failure would provide orthodontists with the most significant bonding information.34
The shear bond strength test is the most commonly
employed in vitro test method for orthodontic bonding on
various surfaces.1,4,13,32,35 However, it is also well known
that due to the heterogeneity of stress distribution over
larger surfaces (>2 mm2), the average stress values become questionable with this test method.43 In addition, the
fracture pattern in shear bond testing may cause cohesive
failures in the substrates, which may lead to misinterpretation of the data.6 On the other hand, the microshear bond
test allows more reliable evaluation of bond strength of
adhesive systems by decreasing the possibility of defects
either on the substrate surface or the tested adhesive. For
this reason, microshear bond strength values are often
higher than macroshear test results.7
6

All
Polished

Fig 3 Means and standard

deviations of SBS values for
the experimental groups as
a function of zirconium oxide
material, surface finish, and
surface conditioning methods.

Achieving durable adhesion of resin-based materials

to zirconium oxide is a challenge. Previous studies clearly
defined that unlike for glass-based ceramics, hydrofluoric
acid etching is not sufficient to bond resin materials to zirconium oxide surfaces.5,20,31 In this study, mechanical retention was attained through air abrasion with either Al2O3
or silica-coated alumina particles. Although some authors
claimed initiation of microcracks as a result of mechanical
abrasion techniques,47,48 other studies showed that mechanical abrasion causes a phase change from tetragonal
to monoclinic, which would in fact resist crack propagation
and flaw-induced decrease in the strength of the material.15,23 Those authors also reported that air abrasion was
more favorable to fine polishing or grinding in terms of
phase change. The present results showed that application of silica-coated alumina particles (CoJet) increased
the bond strength values more than did air abrasion with
Al2O3 particles. Where the latter creates microretentive
sites by increasing surface area and roughness,2,3,31 silica particles not only roughen the surface, they also have
a chemical effect: as a result of blasting pressure, the
embedded silica and alumina particles chemically react
with the silane coupling agent.6 The improved chemical
bonding with silane coupling agents in this approach is
advocated to be the key factor for a higher resin bond
strength when compared to Al2O3 particle air abrasion.6,30
In this study, instead of a conventional silane, a universal
primer was used that has both a silane coupling agent and
methacrylate monomers with functional phosphoric acid
and sulfur compound groups. This might have been the
reason for the high SBS values obtained in the control
group, as zirconium oxide has a high affinity to phosphoric
acid.
The surface finish, whether polished or glazed, significantly affected the bond strength values, except in
the CoJet group. According to surface finish, the control
group (no surface conditioning) showed higher SBS values than Al2O3 for glazed specimens, but for polished
specimens, it was the opposite. For ceramics, it is suggested that removal of the glaze layer increases the
surface area for mechanical retention and allows the
reaction of silane coupling agents with the glassy matrix.35 This is because the presence of glass phase in
The Journal of Adhesive Dentistry

Canigur Bavbek et al

ceramics is known to be conducive to better siloxane

bonds.6 However, in zirconia-based ceramic systems,
the high crystalline content and lack of glass phase (less
than 1%) decrease the probability of establishing a stable chemical bond.6,9,37 In supporting of this statement,
a recent study found the glaze layer on zirconium oxide
surfaces to provided a strong durable bond to resin cement.10 These phenomena may be the reasons for the
results obtained between an undisturbed glaze layer with
concentrated glass particles and the silane agents in
the universal primer in the control glazed group. On the
other hand, air abrasion with Al2O3 particles successfully
eliminated the glaze layer, but it could not act further
on the MZ surface or increase its surface energy to the
extent that CoJet did, which resulted in a lower mean
bond strength value. Notwithstanding, Al2O3 abrasion
enhanced bonding in the polished group, probably due
to better exposure of MZ surface for further reaction with
phosphoric-acid methacrylate and silane.
The average force transmitted to a bracket during
mastication was reported to be 40 to 120 N, and therefore it should be able to resist stress values between 6
and 8 MPa during fixed orthodontic therapy for clinical
success.34 The mean bond strength values of brackets
bonded to natural teeth are significantly lower than those
obtained for surfaces other than enamel, especially when
a chemical promoter such as silane is used during bonding.12 The present results showed that even in the control
group where no surface conditioning was practiced, the
mean bond strength value was 20.3 4.7 MPa to polished surfaces, which was the lowest mean value among
all groups. These results may imply that universal primer
application alone, prior to bonding, would already enhance
the bond strength of the orthodontic resin composite
tested. However, it is known that in vitro bond strength
values are often higher than in clinical situations, and biodegradation of resin composites in the oral environment
over time may even decrease these values.13,27 In addition, in vitro aging procedures have a detrimental effect on
the bond strength values of resin composites when compared to non-aging test conditions.1,10,29 Cochran et al12
stated that bond strength values between 7 and 10MPa
or higher can be acceptable for bracket bonding to porcelain surfaces, if it is determined that surface damage to
the porcelain will not occur during debonding the bracket
at the end of orthodontic treatment.
Microshear bond strength values varied depending on
the surface conditioning method, but failure types were
similar in all groups mainly adhesive failures were observed. Although quite high bond strength values were
achieved after air abrasion with either Al2O3 or CoJet
sand, the results did not exceed the cohesive strength of
zirconium oxide; thus no cohesive failures were observed
in the substrate. This indicates that there was no reliable,
durable chemical bond between the resin composite and
the zirconium oxide surface, which is in line with previous studies in which different test methods were also
used.2,3,5,20,31 With microshear testing, force is applied
as close as possible to the adhesive/substrate interface;
accordingly, debonding forces are more concentrated on
doi: 10.3290/j.jad.a32812

the interface.33 The forces were not sufficient to damage

the MZ substrate, but were capable of interrupting the
integrity of the adhesive resin, which resulted in mixed
type of failures.
The lack of aging procedures must be considered a
limitation of this study. As reported previously, long-term
(two-year) water storage45 or 6000 thermocyles31 decreased the bond strength of bis-GMA resin composites,
regardless of air abrasion or silica coating and silanization. Hence, because no aging was performed in this
study, the results should be carefully and critically evaluated, considering that bonding in orthodontics is semipermanent. However, at least 24-month water storage
should be preferred for orthodontic bond strength testing,28 since it is usually the average period of time for
complete orthodontic treatment with fixed appliances,
and significant decreases may be expected under such
prolonged aging conditions compared to shorter durations of only a few days to several months.13,28 The bond
strength is affected by aging only when a mechanical
pre-treatment is not applied prior to an MDP-containing
primer.46 Wegner and Kern45 also showed that the bond
strength of an MDP-containing resin composite did not
change significantly after aging.45 For this reason, the
use of universal primers containing methacrylated phosphoric acids and silane should be preferred after airabrasion protocols.

CONCLUSIONS
From this study, the following could be concluded:
y Monolithic zirconium oxide type (high purity or yttria
stabilized) did not significantly influence the adhesive
strength of the orthodontic resin composite tested.
y In all groups, the highest mean SBS values were
achieved by air abrasion with CoJet sand followed by
universal primer application. Air abrasion with Al2O3
was better than no treatment on polished surfaces,
but universal primer application alone worked better
for glazed surfaces.
y The most predominant failure type was adhesive,
but air abrasion either with Al2O3 or CoJet increased
the frequency of mixed failures. No cohesive failure
within the composite or zirconium oxide was observed.

ACKNOWLEDGMENT
The authors would like to thank the manufacturers (Glidewell Dental Laboratories, USA, and Zirkonzahn GmbH, Germany) for generous provision of the zirconium oxide ceramics tested.

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Clinical relevance: When bonding fixed orthodontic appliances on monolithic zirconium oxide reconstructions
with orthodontic resin composite, if the surface finish
and material type are not known, successful bonding
could be achieved after air abrasion with silica-coated
alumina particles followed by universal primer application, providing that no cohesive failures were observed
within the composite or the zirconia itself.

The Journal of Adhesive Dentistry