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Effect of Surface Modification on the Bond Strength between

Zirconia and Resin Cement

Ferhan Egilmez, DDS, PhD,1 Gulfem Ergun, DDS, PhD,1 Isil Cekic-Nagas, DDS, PhD,1
Pekka K. Vallittu, DDS, PhD,2 Mutlu Ozcan, DDS, Dr.med.dent., PhD,3 & Lippo V.J. Lassila, DDS, PhD2
Department of Prosthodontics, Gazi University Faculty of Dentistry, Ankara, Turkey
Department of Biomaterials Science and Turku Clinical Biomaterials Centre, Institute of Dentistry, University of Turku, Turku, Finland
Dental Materials Unit, Center for Dental and Oral Medicine—Clinic for Fixed and Removable Prosthodontics and Dental Materials Science,
University of Zurich, Zurich, Switzerland

Keywords Abstract
Y-TZP zirconia; milling residue suspension;
micro push-out bond test; adhesive resin
Purpose: This study aimed to evaluate the micro push-out (μ-PO) bond strength
cement. between zirconia and resin cement after addition of zirconia particles to increase the
surface roughness.
Ferhan Egilmez, Gazi University Faculty of Materials and Methods: Y-TZP zirconia specimens in three experimental groups
Dentistry—Department of Prosthodontics, 8. were subjected to Y-TZP particle deposition via dipping into the milling residue
Cadde 82. Sokak No. 4, Emek, Ankara 06510, suspension at different times prior to the sintering process. The dipping procedure
Turkey. E-mail: ferhanegilmez@gmail.com was repeated twice for each specimen in group B, six times in group C, and ten
times in group D. The specimens subjected to airborne-particle abrasion (110 μm
This study was financed by the Bio- and Nano Al2 O3 , Rocatec Pre) acted as the control group (group A). All of the specimens were
Polymers Research Group, Centre of then bonded using adhesive resin cement (RelyX Ultimate). A μ-PO test was used to
Excellence of the Academy of Finland. determine the bond strength values. One-way ANOVA at a 5% confidence level was
The authors deny any conflicts of interest.
performed for data analysis. Optical microscopy and scanning electron microscopy
(SEM) were used to evaluate the failure modes and surface structure.
Accepted December 27, 2012 Results: Y-TZP particle deposition did not have a significant effect on the bond
strength of the resin cement to zirconia specimens when compared to the control (p =
doi: 10.1111/jopr.12030 0.141). Higher bond strength values were observed in groups C and D than in control.
The surface layer presented blister-like porosities with openings of various diameters
ranging between 2 and 4 μm.
Conclusion: Y-TZP particle deposition after dipping six and ten times did not improve
the mean bond strength statistically but presented surface topography that may be
favorable for increased micromechanical retention for adhesive resin cement.
Clinical Significance: Y-TZP particle deposition may create a more retentive surface
than airborne-particle abrasion for adhesive bonding between zirconia surface and
resin cement.

It is important for dental materials to have not only favorable 1170◦ C and 2370◦ C and cubic above 2370◦ C and up to the
optical properties, but also favorable mechanical and biological melting point.2 Nonetheless, the tetragonal phase may trans-
properties, adequate clinical function, and longevity. Currently, form into monoclinic upon cooling. This phase transforma-
several ceramic materials, including crystalline-dominated tion exhibits approximately a 4.5% volume expansion that
ceramics, glass-based ceramics, and polycrystalline ceramics, leads to catastrophic failure. Alloying pure zirconia with sta-
meet these requirements.1-3 Recently, zirconia has gained in- bilizing oxides such as CaO, MgO, Y2 O3 , or CeO2 has been
creased popularity in contemporary dentistry due to its high shown to maintain the tetragonal structure at room temperature.
biocompatibility, low bacterial surface adhesion, high flexural The advantage of controlling the stress-induced tetragonal-to-
strength, toughness due to transformation toughening mecha- monoclinic phase transformation is to arrest crack propagation
nism, and esthetic properties.4 and achieve high toughness.2
Pure zirconium dioxide possesses three crystallographic The use of partially yttrium-stabilized zirconia (Y-
forms that are stable at a different range of temperatures un- TZP) has been facilitated by the advent of computer-
der atmospheric pressure. The monoclinic phase is stable up aided design/computer-aided manufacturing (CAD/CAM)
to approximately 1170◦ C. The structure is tetragonal between systems.5-7 The milling of semisintered zirconia has the

Journal of Prosthodontics 22 (2013) 529–536 

C 2013 by the American College of Prosthodontists 529
Surface Modification Technique for Improved Bonding to Zirconia Egilmez et al

advantages of shorter milling times and less wear of the cutting pothesis tested was that surface modification of zirconia with
burs, but this technique necessitates a final sintering after the zirconia particles would increase the push-out bond strength of
milling process.8 This sintering procedure is associated with resin cement to zirconia compared to air abrasion.
certain amount of shrinkage. On the other hand, the milling
of fully sintered zirconia, which is processed through hot iso- Materials and methods
static pressing, is another option for manufacturing zirconia
restorations.9 Four groups of specimens were tested for bond strength of resin
A key problem facing dental operators using highly crys- cement to zirconia using the micro push-out (μ-PO) test. The
talline ceramic restorations such as zirconia is the inability to groups were (A) control group, air-abraded with alumina, (B)
etch and silanize the surface to create topography conducive zircona surface treated two times with added zirconia particles
to micromechanical and chemical bonding to dental resin prior sintering to increase the surface roughness, (C) treated six
cements.10 This is mainly because zirconia ceramic contains times, and (D) treated ten times. Surfaces were analyzed using
no silica or any substantial glassy phase in its microstructure.2 stereo microscope and scanning electron microscope (SEM) to
On the other hand, systems such as CoJet and Rocatec (3M detect levels of roughness.
ESPE Dental Products, Seefeld, Germany) were reported to
use mechanical energy (grit-blasting under pressure) to trans- Preparation of zirconia specimens
fer silica-coated alumina particles to the surface of the ceramic
Disk-shaped partially yttrium stabilized green stage zirconia
substrate.11 Furthermore, the subsequent application of silane
specimens (N = 60, n = 15/group) (diameter: 1.5 mm; height:
coupling agent to the silica-coated surface was demonstrated
4 mm) were fabricated (ICE Zirkon Translucent 95H14, Zircon-
to achieve chemical adhesion between polymers and inorganic
zahn, Bruneck, Italy; Batch#: ZB 1230B) using a CAD/CAM
substances, which significantly improves bond strength.12-14
copy-milling system (Zirconzahn). All specimens were ultra-
Also, the combination of silane primers and resin cements that
sonically cleaned (Quantrex 90, L&R Ultrasonics, Kearny, NJ)
contain phosphoric acid in the form of a phosphate monomer
for 10 minutes in ethanol and deionized water in sequence and
(MDP) enhances the adhesion to zirconia ceramics.15 Yet, ini-
air dried. Then, they were randomly allocated to four groups
tial air abrasion was reported to increase the adhesion of MDP-
(groups A to D), where group A acted as the control, and
based cements on zirconia.16,17 However, a disadvantage of
groups B, C, and D were the experimental groups. The diam-
air abrasion is that the aerosol produced is a suspension of
eter of the specimens was determined prior to coating using a
extremely fine (<50 μm) airborne particles in the form of a
digital caliper (Liaoning MEC Group, Dalian, China) with an
liquid, solid, or combinations of both. Aspiration of such small
accuracy of 0.01 mm.
particles is considered to be unhealthy, as they remain in the
Zirconia milling residue was collected from the CAD/CAM
air for a longer time. These particles are capable of penetrating
copy-milling system after the milling process of zirconia
deep into the respiratory tract and could be harmful for both
blanks. Milling residue suspension (MRS) (50 mg/ml) was
patients and operators.18 Additionally, particle abrasion using
prepared by weighting 0.499 g zirconia milling residue and
Al2 O3 or other abrasives with a size ranging from 50 μm to
mixing it in 10 ml of deionized water, using a magnetic
250 μm could create surface micro-cracks and decrease frac-
stirring device to a final volume of 10 ml. Specimens in the
ture strength and apparent fracture toughness of zirconia.19,20
experimental groups were held in stainless steel cotton forceps,
Moreover, it can also result in a tetragonal-to-monoclinic phase
dipped into the MRS, and allowed to air dry for 1 minute. This
change on the surface of zirconia that can theoretically pro-
procedure was repeated twice for each specimen in group B,
duce a compressive stress layer counteracting the flaw-induced
six times in group C, and ten times in group D. All specimens
reduction in strength.19 Thompson et al21 reported that excess
were prepared by the same operator at 22◦ C to 22.5◦ C room
surface grinding could diminish the strength of zirconia.
temperature and relative humidity of 50%. Then, all specimens,
Other studies have suggested the use of phosphate monomers
including the control group, were sintered (Zirkonofen 600,
and modification of zirconia surfaces using the selective infiltra-
Zirkonzahn) at 20◦ C to 1500◦ C at a rising time of 3 hours and
tion technique followed by hydrofluoric acid etching to increase
kept at 1500◦ C for 2 hours according to the manufacturer’s rec-
bond strength values.11,22 Hydrofluoric acid is a poisonous,
ommendation. The thicknesses of the MRS-coated specimens
caustic, foaming liquid extremely dangerous to the skin and
were measured again after the sintering process. The specimen
lungs.23 Other alternative methods for increasing bond strength
surfaces in group A were airborne-particle abraded with
to zirconia is the precipitation of nano-sized alumina crystals
110 μm Al2 O3 particles (Rocatec Pre, 3M ESPE, St. Paul,
on the surface.10 The particles of different ceramic materials
MN) at 280 kPa pressure from a distance of about 10 mm for
may be deposited on the substrate, but the disadvantage of this
20 seconds. All of the specimens (control + experimental)
process is that the coatings are relatively thick, from several
were again ultrasonically cleaned in 96% isopropyl alcohol for
tens of μm to several hundreds of μm. As a result, when sub-
10 minutes.
jected to subsequent thermal treatment, they may crack, and
therefore are not suitable for clinical use.
Luting procedures
The issue of creating an optimal surface that could increase
the bond strength between zirconia and resin cement remains. A putty-silicone (Zetaplus, Zhermarck Badia Polesine, Rovigo,
Therefore, this study’s aim was to evaluate the micro push-out Italy, Batch #: C100600) mold was made. Holes were prepared
bond strength between zirconia and resin cement after adding into the mold using a stainless steel cylinder (diameter: 1.5
zirconia particles to increase the surface roughness. The hy- mm, height: 5 mm). Metal rings (thickness: 1 mm, diameter:

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Egilmez et al Surface Modification Technique for Improved Bonding to Zirconia

Figure 1 Specimen preparation where the resin cement is bonded zirconia surface for the μ-PO test.

5 mm) with openings in their middle were centered onto the were loaded with a cylindrical punch tip (1 mm diameter)
cylindrical holes. All specimens were air dried and pretreated centered on the zirconia surface. Care was also taken to en-
with an adhesive resin (Scotchbond Universal Adhesive, 3M sure the contact between the punch tip and the zirconia spec-
ESPE, Batch #: 452632) as a primer according to the manu- imen was over the most extended area, to avoid notching the
facturer’s recommendation. Then, the specimens were mounted punch tip into the zirconia surface. Loading was performed
into the holes in upright position (Fig 1). Adhesive resin cement at a 0.5 mm/min crosshead speed until the zirconia specimen
(RelyX Ultimate, 3M ESPE, Batch #: 456882) was injected was dislodged from the resin cement. A maximum failure load
around the zirconia specimens and photo-polymerized for 20 value (N) was recorded and converted into MPa considering the
seconds in four directions according to the manufacturer’s in- bonding area (A, mm2 ) of the specimens using the following
structions with an LED polymerization unit (Elipar S10, 3M formula:26
ESPE) with an irradiance of 1200 mW/cm2 . The output of the
Micro push−out bond strength = Maximum failure load (N)/
light was controlled with a radiometer on the polymerization
unit itself. Excess zirconia was cut with a diamond disc (80 μm Adhesion area of the adhesive resin cement (mm2 )
diamond, Cerafil bur; Komet Inc, Lemgo, Germany) in a high-
speed handpiece under air coolant. Excess cement was wiped Because of the cylindrical shape of the cemented specimens,
off, and all the prepared test specimens were ground flat using the bonding area was calculated using the formula:27
silicon carbide abrasive paper up to 1000 grit (Federation of
A = 2πrh
European Producers of Abrasives-FEPA) under running water
cooling (StruersRotoPol 11, Struers A/S, Rodovre, Denmark). where r is the specimen radius, π is the constant 3.14, and h is
the thickness of each specimen.
Push-out bond strength test
Failure type analysis
The push-out technique used in this study allows for reduced
dimension of the specimens, yielding more uniform stress The surface of each debonded specimen and failure modes
distribution.24-27 It provides a better estimation of bond strength were examined using an optical microscope at 40× magnifica-
than the conventional shear test, as fracture occurs parallel and tion (Stereo-microscope, Wild M3B, Heerburg, Switzerland).
not transverse to the bonding interface.28 Failure modes were classified into three categories: adhesive
The adhesive resin cement bond to the modified zirconia sur- failure if the fracture site was located entirely between the resin
face was characterized using the μ-PO test by applying a com- cement and zirconia surface, mixed failure if the fracture site
pressive load to the test specimens via a cylindrical plunger continued into the resin cement, and cohesive failure if the
mounted in the Universal Testing Machine (Lloyd LR 30K fracture occurred exclusively within the resin cement. An addi-
Plus, Lloyd Instruments Ltd., Fareham, UK). The specimens tional two zirconia specimens from each group were prepared

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Surface Modification Technique for Improved Bonding to Zirconia Egilmez et al

Figure 2 Mean μ-PO bond strength values (MPa) in each group. *Vertical error bars show plus or minus one standard deviation from the mean value.

for SEM analysis to evaluate the surface structure. The spec- Nontreated zirconia specimens typically showed a smooth
imens were sputter coated (Bal-Tec SCD 050 Sputter Coater; surface with regularly distributed crystal grains (Figs 3A, 4A).
Bal-Tec, Balzers, Liechtenstein) with gold and observed under Group A (control group) exhibited a surface morphology con-
SEM (JSM-5500; JEOL Ltd., Tokyo, Japan) for the examina- sisting of shallow pits and an edge-shaped micro-rough surface
tion of representative zirconia surfaces after the coating pro- texture with distributed micro-irregularities (Figs 3B, 4B).
cedure at different dipping times. Furthermore, the pore and Zirconia-particle deposited surfaces were highly dense and
grain size determinations of zirconia for each group were made rough (Figs 3C, 3D, 3E, 4C, 4D, 4E). At high magnification,
with SEM (400×) using semiautomatic image analysis for the deposited layer presented many smooth blister-like bubbles
calculation. with voids surrounded by a porous layer with openings of
various diameters. Micro-structured protruding porous surface
texture was seen growing perpendicular to the substrate after
Statistical analysis
the zirconia particle deposition. Figures 3C and 4C show
Statistical analysis of the μ-PO bond strength data were per- the change in surface structure on the substrate surface after
formed using a factorial ANOVA and post hoc Tukey’s tests at zirconia particle deposition in group B. According to the SEM
a 95% significance level (SPSS 14.0, Chicago, IL). Statistical analysis, dipping twice resulted in a small amount of blocked
differences in failure modes were investigated by chi-square pores and seemed to exhibit an interconnected network of pores
tests at a significance level of p < 0.05. (Fig 4C). The ten-time coated surface seemed to be completely
covered by the opened porous protruding layer with large pores
Results (Fig 4E).
Additionally, the coating showed good surface coverage and
Statistical analysis demonstrated that zirconia particle deposi- appeared to tightly adhere to the zirconia substrate. There were
tion did not have a significant effect on the bond strength of no cracks or delaminations within the coating layer and at the
resin cement to zirconia specimens compared with the control coating/substrate interface. The average pore size decreased
(p = 0.141); however, a slight nonsignificant increase in bond with increased numbers of dipping. The pore size ranged be-
strength values was observed in groups C and D (Fig 2). Di- tween approximately 2 μm and 4 μm for group D specimens,
ameter measurements of the specimens prior to coating and being higher than the other groups. As a result, the coating
after the sintering process exhibited similar results. Repeating topography was quite porous in ten-time coated specimens
the coating procedure for different times did not increase the (Figs 3E, 4E), in marked contrast to the twice or six-time
specimen diameter. coated ones (Figs 3C, 3D, 4C, 4D). It was evident that the open

532 Journal of Prosthodontics 22 (2013) 529–536 

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Egilmez et al Surface Modification Technique for Improved Bonding to Zirconia

Figure 3 Representative SEM micrographs of zirconia surfaces in experimental groups. (Original magnification 1000×, bar = 10 μm.) (A) Nontreated
zirconia surface, (B) airborne-particle abraded surface (control), (C) treated two times with added zirconia particles, (D) treated six times, (E) treated
ten times.

Figure 4 Representative SEM micrographs of zirconia surfaces in experimental groups. (Original magnification 4000×, bar = 5 μm). (A) Nontreated
zirconia surface, (B) airborne-particle abraded surface (control), (C) treated two times with added zirconia particles, (D) treated six times, (E) treated
ten times.

porosity of the surface layer increased with the dipping time in cant among the groups (p > 0.05). Optical microscope analysis
MRS prior to the sintering process. demonstrated predominantly mixed failures in all groups.
Figure 5 illustrates the distribution of failure modes in tested
groups: an adhesive failure where the bond interfacial surfaces
are exposed, a mixed mode (failure surface displays areas of Discussion
exposed bonding surface and remnants of resin cement fail- Several surface-conditioning methods based on mechanical or
ure) and cohesive failure (the fracture is purely in the resin chemical modifications including surface grinding, air abrasion,
cement). The difference of the failure modes was not signifi- combination of air abrasion and use of an MDP-containing

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Figure 5 Distributions of failure modes after debonding in each group.

primer/silane, tribochemical silica coating, or the precipita- plication of fused glass micro-pearls to the surface fol-
tion of nano-sized alumina crystals on the zirconia surfaces lowed by silanizaton of zirconia increased TBS of resin ce-
have been used to improve the bond strength of resin to ments to zirconia (14.5 ± 1.1 MPa) when compared to
zirconia.10,21,29 Overall results of the current study indicated the nontreated zirconia (7.5 ± 1.5 MPa). In another study,
that by increasing the treatment time (ten times dipping com- application of a blend of 3-mercaptopropyltrimethoxysilane
pared to two or six times) before the sintering process, the μ-PO and 1,2-bis-(triethoxysilyl)ethane, after alumina particle abra-
bond strengths were higher; however, the results of this study sion, followed by tribochemical silica-coating, created the high-
demonstrated that zirconia specimens with different micro- est SBS (21.9 ± 8.7 MPa) of the two cements to zirconia.32 The
porous surfaces did not significantly affect the μ-PO bond difference in the testing methods for bond strength could be one
strength. Thus, the null hypothesis could be rejected. Although of the causes of such a discrepancy in the current results; how-
the presented technique did not exhibit a statistically significant ever, these values may be potential sources of guidance for the
increase in bond strength results compared to the air-abraded current data.
specimens, it is very important not to cause any adverse effect According to the SEM analysis, two dipping times had a
on the zirconia surface by means of creating microcracks and small amount of blocked pores and seemed to exhibit an inter-
producing phase change. Nevertheless, the effects of storage connected network of pores. Similar bond strength results were
conditions (i.e., storage times, solutions, or temperature) that obtained in this group (B), which were lower than the control.
would have a detrimental effect on the bond strength were not Nevertheless, with the increased number of dipping processes,
evaluated in this study. Furthermore, it would appear appropri- the pores on the outer surface gradually became greater, and
ate to use the same technique with a variety of resin cements, as the ten-time coated surface seemed to be completely covered
only one cement was selected in this study. Also, the application by the opened porous protruding layer. The pores were larger
of other chemical or mechanical surface conditioning methods in group D specimens dipped into MRS ten times. The aver-
as controls would be beneficial for evaluating the efficiency of age pore size decreased with an increasing number of dipping
the current experimental design. processes. In this way, a large micro-retentive area was created
Other studies focusing on surface modification of the inert on the zirconia substrate, with the potential for promoting resin
surfaces of zirconia demonstrated comparable bond strength bonding. From SEM micrographs (Figs 3E, 4E), it is clear that
values. Aboushelib et al30 showed that using selective infil- the same holds true for the coatings deposited on the zirconia
tration technique on zirconia surfaces resulted in increased substrates. In addition, it should be pointed out that with this
μ-TBS (49.8 ± 2.7 MPa) when compared with air-particle novel technique, not only was an irregular surface topography
abrasion (33.4 ± 2.1 MPa). By using this technique, im- and protruding micro-porous layer with opened morphology
proved nano-mechanical retention of zirconia was obtained and surface coverage obtained, but also it had no effect on the
by increasing the surface area available for bonding. On thickness of the sintered substrate. Furthermore, after the sin-
the other hand, Kitayama et al31 demonstrated that the ap- tering process, it was evident that the coating-substrate contact

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Egilmez et al Surface Modification Technique for Improved Bonding to Zirconia

was firm, and the coating could not be removed from the sub- References
strate, indicating the formation of stronger bonds between the
substrate and coating. 1. Olsson KG, Fürst B, Andersson B, et al: A long-term
The SEM findings gave a view on the protruded micro-porous retrospective and clinical follow-up study of In-Ceram Alumina
FPDs. Int J Prosthodont 2003;16:150-156
structure of the Y-TZP substrates and the distribution of pores.
2. Denry I, Kelly JR: State of the art of zirconia for dental
It also revealed that the pore size ranges from approximately applications. Dent Mater 2008;24:299-307
2 μm to 4 μm, which could support the increased bond strength 3. Raigrodski AJ, Hillstead MB, Meng GK, et al: Survival and
results of the current study. At this point, the authors speculate complications of zirconia-based fixed dental prostheses: a
that due to this micro-porosity, an adhesive layer might have systematic review. J Prosthet Dent 2012;107:170-177
been formed by the codeposition of zirconia powders while the 4. Guess PC, Att W, Strub JR: Zirconia in fixed implant
open porosity of the surface layer was increased with the dip- prosthodontics. Clin Implant Dent Relat Res 2012;14:633-645
ping time to the MRS prior to the sintering process. Moreover, 5. Raigrodski AJ, Chiche GJ, Potiket N, et al: The efficacy of
the resin matrix may have filled all the opened pores and flowed posterior three-unit zirconium-oxide-based ceramic fixed partial
around the blister-like, semispherical zirconia particles form- dental prostheses: a prospective clinical pilot study. J Prosthet
Dent 2006;96:237-244
ing an intermediate structure designated as the hybrid layer.
6. Vigolo P, Fonzi F: An in vitro evaluation of fit of
Subsequently, penetration of the resin cement into pores in the zirconium-oxide-based ceramic four-unit fixed partial dentures,
MRS-coated surface of the specimens provides micromechan- generated with three different CAD/CAM systems, before and
ical retention, which has been considered to establish a strong after porcelain firing cycles and after glaze cycles. J Prosthodont
and durable resin to zirconia bond. It should also be noted that 2008;17:621-626
only one resin cement was used in the current study because of 7. Vigolo P, Motterle M: An in vitro evaluation of zirconia surface
the simplicity and proof of the principle; however, this does not roughness caused by different scaling methods. J Prosthet Dent
represent all resin cements. 2010;103:283-287
In this study, a new adhesive resin cement containing MDP 8. Beuer F, Schweiger J, Edelhoff D: Digital dentistry: an overview
was used to evaluate bond strength to zirconia. Higher bond of recent developments for CAD/CAM generated restorations. Br
Dent J 2008;204:505-511
strength results were obtained previously by using the combina-
9. Alghazzawi TF, Liu PR, Essig ME: The effect of different
tion of silane primers and resin cements that contain phosphoric fabrication steps on the marginal adaptation of two types of
acid and MDP.14 In the current study, however, failure mode ob- glass-infiltrated ceramic crown copings fabricated by CAD/CAM
servations revealed that the majority of failures had remaining technology. J Prosthodont 2012;21:167-172
resin cement material still adhered to the zirconia. This might 10. Everson P, Addison O, Palin WM, et al: Improved bonding of
be the result of a benefit from both surface modifications with zirconia substructures to resin using a “glaze-on” technique. J
zirconia particle deposition and chemical functionalization of Dent 2012;40:347-351
the surface. Hence, zirconia particle deposition may also create 11. Senyilmaz DP, Palin WM, Shortall AC, et al: The effect of
a retentive surface as airborne-particle abrasion for adhesive surface preparation and luting agent on bond strength to a
bonding between zirconia surface and resin cement and could zirconium-based ceramic. Oper Dent 2007;32:623-630
12. Valandro LF, Della Bona A, Antonio Bottino M, et al: The effect
be an alternative method to condition zirconia surfaces for clin-
of ceramic surface treatment on bonding to densely sintered
ical applications. alumina ceramic. J Prosthet Dent 2005;93:253-259
Future studies are required to examine the impact of increas- 13. Derand T, Molin M, Kvam K: Bond strength of composite luting
ing dipping time on μ-PO bond strength. Furthermore, using cement to zirconia ceramic surfaces. Dent Mater
this technique with a variety of resin cements or the compari- 2005;21:1158-1162
son of the technique with other chemical or mechanical surface 14. Ernst CP, Cohnen U, Stender E, et al: In vitro retentive strength
conditioning methods or long-term fatigue simulation would of zirconium oxide ceramic crowns using different luting agents.
appear to be sensible to provide an indication of likely clinical J Prosthet Dent 2005;93:551-558
performance. 15. Matinlinna JP, Heikkinen T, Özcan M, et al: Evaluation of resin
adhesion to zirconia ceramic using some organosilanes. Dent
Mater 2006;22:824-831
16. Özcan M, Kerkdijk S, Valandro LF: Comparison of resin cement
adhesion to Y-TZP ceramic following manufacturers’
Conclusions instructions of the cements only. Clin Oral Investig
From this in vitro study, the following conclusions were
17. Özcan M, Nijhuis H, Valandro LF: Effect of various surface
drawn: conditioning methods on the adhesion of dual-cure resin cement
1. Zirconia particle deposition using CAD/CAM zirconia with MDP functional monomer to zirconia after thermal aging.
milling residue suspension created micro-structures of Dent Mater J 2008;27:99-104
18. Roeters JJ: A simple method to protect patient and environment
ultrathin protruding porous texture on the zirconia sur-
when using sandblasting for intraoral repair. J Adhes Dent
face compared to airborne particle abrasion. 2000;2:235-238
2. Zirconia particle deposition did not have a significant 19. Kosmac T, Oblak C, Jevnikar P, et al: The effect of
effect on the bond strength of resin cement to zirconia surface grinding and sandblasting on flexural strength and
specimens compared with the air-abraded control group reliability of Y-TZP zirconia ceramic. Dent Mater 1999;15:
(p = 0.141). 426-433

Journal of Prosthodontics 22 (2013) 529–536 

C 2013 by the American College of Prosthodontists 535
Surface Modification Technique for Improved Bonding to Zirconia Egilmez et al

20. Kosmac T, Oblak C, Jevnikar P, et al: Strength and reliability of 27. Egilmez F, Ergun G, Cekic-Nagas I, et al: Influence of cement
surface treated Y-TZP dental ceramics. J Biomed Mater Res thickness on the bond strength of tooth-colored posts to root
2000;53:304-313 dentin after thermal cycling. Acta Odontol Scand
21. Thompson JY, Stoner BR, Piascik JR, et al: 2013;71:175-182
Adhesion/cementation to zirconia and other non-silicate 28. Kienanen P, Alander P, Lassila LV, et al: Bonding of ceramic
ceramics: where are we now? Dent Mater 2011;27:71-82 insert to laboratory particle filler composite. Acta Odontol Scand
22. Aboushelib MN, Mirmohamadi H, Matinlinna JP, et al: 2005;63:272-277
Innovations in bonding to zirconia-based materials. Part II: 29. Özcan M, Vallittu PK: Effect of surface conditioning methods on
focusing on chemical interactions. Dent Mater 2009;25:989-993 the bond strength of luting cement to ceramics. Dent Mater
23. Özcan M, Allahbeickaraghi A, Dundar M: Possible hazardous 2003;19:725-731
effects of hydrofluoric acid and recommendations for treatment 30. Aboushelib MN, Kleverlaan CJ, Feilzer AJ: Selective
approach: a review. Clin Oral Investig 2012;16:15-23 infiltration-etching technique for a strong and durable bond of
24. Cekic-Nagas I, Ergun G, Nagas E, et al: Comparison between resin cements to zirconia-based materials. J Prosthet Dent
regional micropush-out and microtensile bond strength of resin 2007;98:379-388
composite to dentin. Acta Odontol Scand 2008;66:73-81 31. Kitayama S, Nikaido T, Maruoka R, et al: Effect of an
25. Castellan CS, Santos-Filho PC, Soares PV, et al: Measuring bond internal coating technique on tensile bond strengths of resin
strength between fiber post and root dentin: a comparison of cements to zirconia ceramics. Dent Mater J 2009;28:
different tests. J Adhes Dent 2010;12:477-485 446-453
26. Egilmez F, Ergun G, Cekic-Nagas I, et al: Bond strength of 32. Matinlinna JP, Lassila LV, Vallittu PK: Pilot evaluation of resin
self-adhesive resin cements to dentin after antibacterial and composite cement adhesion to zirconia using a novel silane
chelating solution treatment. Acta Odontol Scand 2013;71:22-31 system. Acta Odontol Scand 2007;65:44-51

536 Journal of Prosthodontics 22 (2013) 529–536 

C 2013 by the American College of Prosthodontists