Stability of the bond between two resin

cements and an yttria-stabilized zirconia

ceramic after six months of aging in water
Eduardo M. da Silva, DDS, MSc, PhD,a
Luciana Miragaya, DDS, MSc,b
Carlos Eduardo Sabrosa, DDS, MSc, PhD,c and
Lucianne C. Maia, DDS, MSc, PhDd
School of Dentistry, Federal Fluminense University, Niterói, Rio de
Janeiro, Brazil; School of Dentistry, Rio de Janeiro State University,
Rio de Janeiro, Brazil; School of Dentistry, Federal University of Rio
de Janeiro, Rio de Janeiro, Brazil
Statement of the problem. The behavior of the luting cement and the cementation protocol are essential in the clinical
success of ceramic restorations.

Purpose. The purpose of this study was to evaluate the bond stability of 2 resin cements and a yttria-stabilized tetragonal
polycrystalline zirconia (Y-TZP) ceramic submitted to 2 surface treatments.

Material and methods. Sixty plates of a Y-TZP ceramic were assigned to 3 groups according to the surface treatments: control,
as sintered surface; methacryloxydecyl dihydrogen phosphate (MDP), coated with an MDP-based primer, and tribochemical
silica-coating (TSC), coated with tribochemical silica. The plates of each group were further divided into 2 subgroups according
to the resin cement as follows: RelyX adhesive resin cement (conventional) and RelyX Unicem (self-adhesive). Cylinders of resin
cements (B¼0.75 mm  0.5 mm in height) were built up on the ceramic surfaces, and the plates stored in distilled water at
37 C for either 24 hours or 6 months before being submitted to a microshear bond strength test. The data were submitted to
3-way ANOVA and the Tukey honestly significant difference test (a¼.05).

Results. Three-way ANOVA showed statistical significance for the 3 independent factors: resin cement, surface treatment,
and period of water immersion (P<.001). Unicem presented the highest microshear bond strength after 24 hours (MDP,
37.4 2.3 and TSC, 36.2 2.1 MPa). Except for RelyX adhesive resin cement applied on ceramic surfaces treated with TSC,
the microshear bond strength of all the other groups decreased after 6 months of aging in water. The microshear bond
strength decreased most in the control groups (81.5% for ARC and 93.1% for Unicem). In the group treated with TSC, the
microshear bond strength for Unicem decreased by 54.8% and in that treated with MDP-based primer by 42.5%. In the
group treated with MDP-based primer, the microshear bond strength for RelyX ARC decreased by 52.8%.

Conclusions. Irrespective of surface treatments, self-adhesive resin cement was not able to maintain the bond to Y-TZP
ceramic after 6 months of aging in water. (J Prosthet Dent 2014;112:568-575)

Clinical Implications
Self-adhesive resin cement does not produce a stable bond to
yttria-stabilized tetragonal polycrystalline zirconia ceramic. Tribochemical
silica coating seems to be a more reliable surface treatment for achieving
stability in the bond between conventional resin-based cement and
yttria-stabilized tetragonal polycrystalline zirconia ceramic.

a
Associate Professor, Analytical Laboratory of Restorative Biomaterials (LABiom-R), School of Dentistry, Federal Fluminense University.
b
Doctoral student, Analytical Laboratory of Restorative Biomaterials (LABiom-R), School of Dentistry, Federal Fluminense University.
c
Adjunct Professor, Department of Restorative Dentistry, School of Dentistry, Rio de Janeiro State University.
d
Professor, Department of Pediatric Dentistry and Orthodontics, School of Dentistry, Federal University of Rio de Janeiro.

The Journal of Prosthetic Dentistry da Silva et al

September 2014 569
Establishing a hydrolytically stable achieve strong and reliable bond strength stability of 2 resin cements, RelyX adhe-
bond interface between dental tissues with resin-based cements. In this field, sive resin cement (conventional) (3M
and dental ceramics is one of the most some researchers have shown positive ESPE) (ARC) and RelyX Unicem (self-
important challenges involved in the results with adhesive resin cements on adhesive) (3M ESPE) (UCem) and a
clinical longevity of indirect ceramic airborne-particleeabraded Y-TZP fixed Y-TZP dental ceramic (Lava Frame zir-
restorations.1 At present, the clinical prostheses.31 conium oxide; 3M ESPE). The use of a
protocol most frequently used for luting Although previous studies showed microshear bond strength test and the
ceramic restorations involves dissolving that these strategies increase the bond determination of sample size was based
the glass phase of the ceramic structure strength between Y-TZP dental ceramics on similar previous studies that used
by etching it with hydrofluoric acid and and resin-based cements,14,19,26,32 a similar methodology.8,14,37 Based on
the formation of a network between recently published review article13 these, no preliminary power analysis was
the dispersed silica on the ceramic sur- concluded that the behavior of available performed. The materials composition is
face and the silanol group contained in materials and techniques is still not shown in Table I.
bifunctional primers from a silane cou- predictable in clinical practice. More- Presintered Y-TZP ceramic blocks
pling agent applied after acid etching.2 over, little information is available on (Lava Frame zirconium oxide) were
This mechanism produces a micro- the durability33,34 of the adhesive in- sectioned with a diamond disk (Isomet
retentive surface with high free energy terfaces produced by these methods or 1000; Buehler) to produce 60 ceramic
that increases the interaction between on the outcomes of self-adhesive resin plates that measured 1081.5 mm.
the ceramic, bifunctional primers, and cement evaluations.19,35,36 Therefore, After being sintered according to the
the resin cement.3 To simplify the luting the purpose of this study was to evaluate manufacturer’s instructions, the plates
procedures for ceramic restorations, the hydrolytic stability of the bond were ultrasonically agitated in distilled
manufacturers have developed self- strength between 2 resin cements and an water and divided into 3 groups (n¼20),
adhesive cements that contain adhesive Y-TZP dental ceramic pretreated with according to the following surface
phosphate methacrylate monomers in silica coating or an methacryloxydecyl treatments: control, as sintered surface;
their compositions.4-6 Previous studies dihydrogen phosphate (MDP)-based MDP, the ceramic surfaces were coated
have shown that these monomers can primer. The null hypothesis was that, with a thin layer of Alloy Primer (Kur-
react with the ceramic surface without irrespective of surface treatment, self- aray); and tribochemical silica-coating
any pretreatment, which provides a adhesive resin cement would maintain (TSC), the ceramic surfaces were condi-
bond strength equal to or higher than its bond strength to Y-TZP ceramic after tioned with Rocatec Soft (3M ESPE),
the bond strength produced by conven- 6 months of aging in water. 30 mm silica-modified aluminum oxide
tional resin cements.7,8 (Al2O3) at a pressure of 0.28 MPa for
In the past few years, new reinforced MATERIAL AND METHODS 12 seconds at a distance of 10 mm, fol-
ceramic materials based on yttria- lowed by a layer of ESPE Sil (3M ESPE).
stabilized tetragonal polycrystalline zir- This study investigated the influence The ceramic plates of each group
conia (ZrO2) (Y-TZP) have become of 2 surface treatments on the bond were further divided into 2 subgroups
available to dental clinicians.9 These ma-
terials present high mechanical properties Table I. Composition of materials used
and favorable optical behavior, which
allows them to be used as a framework for Material Manufacturer Composition Batch No.
all types of indirect ceramic restorations,
RelyX ARC 3M ESPE Bis-GMA, TEGDMA, zirconia filler, GEHF
for example, complete crowns, veneers, silica filler, dimethacrylate-polymer
onlays, and fixed dental prostheses.10,11 functionalized, amine, initiator,
However, because of the limited glass peroxide, BP, pigment
phase and the absence of silica in their RelyX Unicem 3M ESPE Powder: glass fillers, silica, calcium 295078
structure, these materials are not suscep- hydroxide, self-polymerizing initiators,
tible to hydrofluoric acid etching and the pigments, light-polymerizing initiators;
liquid: methacrylated phosphoric esters,
formation of a siloxane network with the dimethacrylates, acetate, stabilizers,
silanol groups contained in bifunctional self-polymerizing initiators,
primers.12,13 Based on this finding, re- light-polymerizing initiators.
searchers have proposed different ap- Alloy Primer Kuraray 10-MDP, VBATDT 00257B
proaches, such as silica coating,14-18 the ESPE-Sil 3M ESPE 3-methacryloxyprophyltrimethoxy 332 200
use of phosphate acidic monomers on silane in ethanol
cements or primers,19-24 airborne-particle
BisGMA, bisphenol A glycidyl methacrylate; TEGDMA, triethylene glycol dimethacrylate; BP,
abrasion,25-27 and other techniques28-30 benzoyl peroxide; 10-MDP, 10-methacryloxydecyl dihydrogen phosphate; VBATDT,
to modify the Y-TZP ceramic surfaces to 6-(4-vinylbenzyl-n-propyl) amino-1,3,5-triazine-2,4-dithione.

da Silva et al
570 Volume 112 Issue 3
(n¼10), according to the resin cements cements, and mixed failure (failure at Manugistics). The mSBS data were
used: UCem and ARC. Four polyvinyl ceramic surfaces that included cohe- analyzed by 3-way ANOVA (resin
chloride (PVC) tubes (Embramed) with sive failure of the neighboring resin cement vs surface treatment vs period
an internal diameter of 0.75 mm and a cement). The specimens that debonded of water immersion), followed by serial
height of 0.5 mm were fixed to each spontaneously during the aging in water 2-way and 1-way ANOVAs at each level
ceramic plate surface, and freshly mixed and before the mSBS test were consid- of the study and the Tukey honestly
amounts of each resin cement were ered adhesive failures. Six additional significant difference post hoc test. For
inserted into the PVC tubes with a sy- Y-TZP ceramic plates were divided into 3 specimens that debonded spontane-
ringe with a thin elongated tip (Centrix; groups (n¼2) according to the surface ously during aging in water, the value
3M ESPE). The PVC tubes were covered treatments tested. After treatment, the zero was considered for statistical
with a glass slide and pressed by hand plates were mounted onto aluminum analysis.38 The analysis was performed
to squeeze out the excess material. The stubs, sputter coated with gold- at a significance level of a¼.05.
resin cements were light polymerized for palladium (Au-Pd) (EMITECH model
60 seconds with an irradiance of 1000 K550; Emitech), and observed by scan- RESULTS
mW/cm2 (Elipar Freelight 2 LED Curing ning electron microscope (SEM) (JSM
Light; 3M ESPE). After 30 minutes at 5310; JEOL), which was operated in the Three-way ANOVA (Table II)
room temperature, the PVC tubes were secondary electron and energy dispersive showed statistical significance for the
removed with a scalpel, which exposed spectroscopy (EDS) modes. independent factors of resin cement,
the resin cement cylinders (0.75 mm The statistical analysis was per- surface treatment, and period of water
diameter, 0.5 mm high) bonded to the formed with software (Statgraphics 5.1; immersion (P<.001). The three 2-way
ceramic surfaces. After this, the resin
cement cylinders were checked by ster-
Table II. Summary of 3-way ANOVA and serial 2-way ANOVAs
eomicroscopy at 10 magnification
(FZ40; Olympus) to eliminate those Sum of Mean
with apparent interfacial defects. All the Source of Variation Squares df Square F P
specimens were immersed in distilled
water at 37 C. Resin cement 2324.04 1 2324.04 561.36 <.001
For each experimental group, half of Surface treatment 2445.05 2 1222.52 295.29 <.001
the plates were tested after 24 hours Time 1666.58 1 1666.58 402.55 <.001
and the remaining plates were tested
Resin cement  surface treatment 429.525 2 214.762 51.87 <.001
after 6 months of aging in water. Dur-
Resin cement  time 733.321 1 733.321 177.13 <.001
ing this period, the water was changed
weekly. The ceramic plates were attached Surface treatment  time 104.475 2 52.2377 12.62 <.001
to the testing device (ODMT03d; Odeme Cement  surface treatment  time 38.8632 2 19.4316 4.69 .014
Biotechnology) with cyanoacrylate resin Residual 198.722 48 4.14003
(Super Bonder Loctite; Henkel) and Total 7940.58 59
placed in a universal testing machine
Resin cement 2324.04 1 2324.04 45.77 <.001
(Emic DL 2000; EMIC Equipment and
Test Systems Ltda) with a 50-N load cell. Surface treatment 2445.05 2 1222.52 24.08 <.001
A Kevlar thread (0.2 mm in diameter) Resin cement  surface treatment 429.525 2 214.762 4.23 .020
was looped around the resin cement Residual 2741.97 54 50.7771
cylinders, and a shear force was applied Total 7940.58 59
at a crosshead speed of 1.0 mm/min
Resin cement 2324.04 1 2324.04 40.46 <.001
until failure occurred. The microshear
bond strength (mSBS) value (MPa) for Time 1666.58 1 1666.58 29.01 <.001
each specimen (ceramic plate) was Resin cement  time 733.321 1 733.321 12.77 <.001
considered as the mean obtained from Residual 3216.63 56 57.4399
the 4 resin cement cylinders. Total 7940.58 59
After the mSBS testing, all the speci-
Surface treatment 2445.05 2 1222.52 17.73 <.001
mens were viewed by stereomicroscopy
at 40 magnification (FZ40) to assess Time 1666.58 1 1666.58 24.16 <.001
the failure mode of the resin cement Surface treatment  time 104.475 2 52.2377 0.76 .474
cylinders, according to the following Residual 3724.47 54 68.9717
criteria: adhesive failure at ceramic sur- Total 7940.58 59
faces, cohesive failure in the resin
The Journal of Prosthetic Dentistry da Silva et al
September 2014 571
interactions (P<.001) as well as the Table III. Summary of serial 1-way ANOVAs at each level of interacting factor
3-way interaction (P¼.014) also
showed statistical significance. Serial Source of Variation Sum of Squares df Mean Square F P
2-way ANOVAs (Table II) showed a
Resin cement 2324.04 1 2324.04 24.00 <.001
significant interaction between resin
Within groups 5616.54 58 96.8369
cement and the surface treatment
(P¼.020) and resin cement and the Total 7940.58 59
period of water immersion (P<.001). In Time 1666.58 1 1666.58 15.41 <.001
contrast, the interaction of surface Within groups 6274.0 58 108.172
treatment and period of water immer-
Total 7940.58 59
sion was not significant (P¼.474). One-
way serial ANOVAs (Table III) showed Surface treatment 2445.05 2 1222.52 12.68 <.001
statistical significance for each inde- Within groups 5495.53 57 96.4128
pendent factor (P<.001). Total 7940.58 59
The results of the Tukey honestly
significant difference test as regards
mean comparisons are presented in
Figure 1. UCem presented the highest 45
24 h
mSBS values on ceramic surfaces treated 40 a
a
6 mo
with MDP-based primer and TSC after
24 hours of water immersion. The 35
control groups of both resin-based ce- 30
µSBS (MPa)

ments presented the lowest mSBS value

25
results after 6 months of aging in water. c b
The percentage changes in mSBS after 20 c
c
aging in water are shown in Table IV.
15
Except for the group with ARC applied d,e d
on Y-TZP ceramic surfaces treated with 10 e
f
TSC, the mSBS decreased after 6
5 g
months of aging in water in all groups. g
For both resin cements, the control 0
ARC-C
ARC-MDP
ARC-TSC
UCem-C
UCem-MDP
UCem-TSC

ARC-C
ARC-MDP
ARC-TSC
UCem-C
UCem-MDP
UCem-TSC
group showed the highest decrease
in mSBS (81.5% for ARC and 93.1%
for UCem). For UCem, there was a
decrease of 54.8% in ceramic surfaces
1 Bar graphs of microshear bond strength means.
treated with TSC and 42.5% in ceramic Bars with identical letters do not differ statistically
surfaces treated with MDP-based (Tukey honestly significant difference, a¼.05).
primer. In the group treated with
MDP-based primer, a decrease of
52.8% in mSBS was shown for ARC.
The failure mode distribution (Fig. 2) Table IV. Percentage changes in mSBS after aging in water
showed that, except for the UCem
specimens applied to ceramic surfaces
mSBS after mSBS After % Changes in
treated with MDP-based primer and 24 h Water 6 mo of Aging mSBS After
TSC and tested after 24 hours, which Resin Surface Immersion in Water 6 mo of Aging
presented predominantly cohesive fail- Cement Treatment (MPa) (MPa) in Water
ures, all the other groups presented
total adhesive failures. ARC Control 5.4 1.8 1.0 0.8 81.5
Shown in Figure 3 are representa- UCem Control 16.0 1.7 1.1 1.7 93.1
tive EDS spectra and SEM images of ARC MDP 15.9 5.0 8.4 0.4 52.8
Y-TZP ceramic surfaces submitted to UCem MDP 36.2 2.1 15.4 0.9 42.5
3 surface treatments. (A) as sintered ARC TSC 10.0 1.7 11.3 0.7 þ13.0
ceramic surface, showing a high den-
UCem TSC 37.4 2.3 20.5 1.0 54.8
sity of sintered grains of ZrO2; (B) no
relevant modifications on a ceramic mSBS, microshear bond strength; ARC, adhesive resin cement; UCem, Unicem.

da Silva et al
572 Volume 112 Issue 3
100 in good agreement with those of pre-
90 vious studies and reinforce the difficulty
80 of establishing a reliable bond between
70
60
resin-based cements and as-sintered
(%)
50 Y-TZP surfaces.17,19,25,28,32,33,38 This crit-
40 ical barrier to the bonding phenomenon
30 could be associated with the poor
20
wettability of nontreated Y-TZP ceramic
10
0 surfaces.22,29
C MDP TSC C MDP TSC C MDP TSC C MDP TSC In the present study, UCem did not
UCem ARC UCem ARC maintain the stability of the bond to
24 h 6 mo the Y-TZP ceramic after 6 months of
Adhesive Cohesive Mixed aging in water. This finding is sup-
ported by a previous study and led to
2 Failure mode distribution. the rejection of the null hypothesis that,
irrespective of surface treatment, self-
surface coated with MDP-based primer; conflicting reports, long-term water adhesive resin cement would maintain
(C) peaks of silicon (Si) and aluminum storage only was used as an aging the bond strength to the Y-TZP ceramic
(Al) in an EDS spectrum and white method in the present study. after 6 months of aging in water.37 By
areas, which suggests inclusions of After 24 hours of water immersion, contrast, after 6 months of aging in
silica particles on a ceramic surface the mSBS values (rounded) of UCem water, the values of the mSBS of UCem
coated with tribochemical silica. were 2 and 3 times higher than those of in surfaces treated with MDP-based
ARC (Fig. 1). These results are in good primer and TSC were approximately
DISCUSSION agreement with previous studies5,19 and twice those of ARC. This could mean
could prove that the methacrylated phos- that UCem is more reliable than ARC
In the present study, the stability of phoric acid esters in the UCem formula- for luting Y-TZP ceramic restorations.
the bond between a Y-TZP ceramic tion can establish some type of chemical Because other published studies showed
previously submitted to 2 different sur- interaction with Y-TZP ceramic sur- that UCem maintained the bond sta-
face treatments and 2 resin cements, faces.14,21,33 This probable bond mecha- bility with ZrO2 ceramics after aging
UCem and ARC, was evaluated. A nism can be explained by the chemical in water and/or thermocycling,19,34-36
control negative group (as sintered interaction at the interfacial grain level the findings of the present study were
surfaces without any treatment) also between the 2 phosphate groups in somewhat surprising. Some of the dis-
was used in the experimental protocol. methacrylated phosphoric acid esters similarities among the research pro-
The rationale for this was to increase and the hydroxyl groups of the passive tocols used in the mentioned studies
the power of analysis of the results after ZrO2 coating on the Y-TZP ceramic.14,25 and the one used in the present study
6 months of aging in water. The need When analyzing the overall mSBS could explain these discrepancies.
for some kind of artificial aging to results after 24 hours of water immer- In the study by de Souza et al,35 no
simulate the conditions of the oral sion for ARC, the mSBS values were reduction in the mSBS was shown be-
environment in laboratory studies is higher in surfaces treated with a MDP- tween UCem and a Y-TZP ceramic
well established. Long-term water stor- based primer (Fig. 1), whereas, for treated with a MDP-based primer after
age, thermocycling, or a combination UCem, no statistical difference in the incubation in deionized water at 37 C
of both are the most common mSBS values was found between the for 60 days and thermocycled for 5000
methods.18,36,39,40 Although thermocy- 2 ceramic surface treatments (MDP- cycles (5 C-55 C with a dwell time of
cling seems to be a more reliable based primer and TSC). Therefore, it is 30 seconds); in other words, 1523
method of aging, contradictory results reasonable to speculate that the initial hours of water immersion. In the same
have been reported. In other words, power of the chemical interaction pro- way, Luthy et al36 found no differences
although some studies have shown a duced by the methacrylated phosphoric in UCem SBS before and after water
decrease in bond strength after ther- acid ester present in the UCem formu- thermocycling for 333 hours (100 000
mocycling,39 others have shown either lation had overcome the influence of cycles, 5 C-55 C). The specimens used
no effect or an increase.18,36 Moreover, these ceramic surface treatments on the by these researchers were cylindrical,
a recent review study has shown that a mSBS.The control group of both resin stainless-steel rods (3 mm in diameter)
standardized protocol for thermocy- cements presented the highest decrease bonded to the airborne-particleeabraded
cling that permits comparisons across in mSBS after 6 months of aging in surfaces of a ZrO2 -TZP ceramic. More
different studies in laboratory in- water (81.5% for ARC and 93.1% recently, Yang et al19 also found no
vestigations is lacking.40 Based on these for UCem) (Table IV). These results are differences in TBS between UCem
The Journal of Prosthetic Dentistry da Silva et al
September 2014 573
Spectrum 1
Zr
Au

O Au
Zr Au Au Au Au Au Zr Zr
0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20
Full Scale: 2027 cts; Cursor: –0.018 (984 cts) keV A
Zr Spectrum 1
Au

O Au
Zr Au Au Au Au Au Zr Zr
0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20
Full Scale: 577 cts; Cursor: 0.010 (1321 cts) keV B
Zr Spectrum 1
Au

AI
Au
Si

Zr Au AuAu Au Au Zr Zr
0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20
Full Scale: 253 cts; Cursor: –0.033 (475 cts) keV C
3 Representative SEM images and EDS spectra of yttria-stabilized tetragonal polycrystalline ceramic
surfaces submitted to 3 surface treatment. A, As sintered. B, Coated with MDP-based primer. C, Coated
with tribochemical silica. SEM, scanning electron microscope; EDS, energy dispersive spectroscopy; MDP,
methacryloxydecyl dihydrogen phosphate; O, ; Au, gold; Zr, zirconium; Al, aluminum; Si, silicon.

and an Y-TZP ceramic submitted to water may have had more time to thereby facilitating the degradation of
airborne-particle abrasion and MDP- diffuse through the Y-TZP ceramice this structure during 4320 hours of im-
based primer after 150 days of storage UCem interfaces. Furthermore, the mersion in water.18,23,35
in water at 37 C (3600 hours). These smaller diameter of the specimens used The studies of Liu et al8 and Vrochari
researchers also used specimens that here (0.75 mm) may have allowed water et al6 may be used to reinforce this
measured 3 mm in diameter. In the to penetrate the entire Y-TZP ceramice possibility. The researchers showed
present study, because the specimens UCem interfaces. These 2 factors acting that some self-adhesive resin cements
were aged in water for a period of synergically could have increased the (including UCem) presented higher
6 months, a total of 4320 hours, the hydrolysis of the adhesive polymer, water sorption and solubility than
da Silva et al
574 Volume 112 Issue 3
conventional resin cements and stated contrast, as shown in Table IV, ARC to maintain the bond to the Y-TZP
that, although self-adhesive resin ce- was able to maintain the bond stability ceramic after 6 months of aging in water.
ments are recognized as resin-based to tribochemically silica-coated Y-TZP 2. Even losing half of its initial bond
materials, they may be more prone to ceramic surfaces after 6 months. This strength in surfaces treated with MDP-
hydrolytic degradation. Self-adhesive ce- behavior can be explained by the in- based primer or coated with tri-
ments present an acid-based polymeri- crease in roughness, surface area, and bochemical silica after 6 months of
zation reaction component because their free energy of the ceramic surfaces aging in water, UCem presented bond
characteristics are similar to modified produced by abrasion with silica- strength twice that of ARC. This could
glass ionomer cement and because they modified Al2O315,20,25 and by the sil- be interpreted as UCem being more
contain large numbers of hydrophilic ica layer becoming embedded in the reliable than ARC for luting Y-TZP
functional groups. The failure mode dis- ceramic surface, which increases its ceramic restorations
tribution (Fig. 2) would seem to reflect wettability. The increase in Si content, 3. Although recent studies have
this phenomenon; that is, although the shown in the energy dispersive x-ray proposed the use of metal primers, for
UCem specimens of the MDP and TSC spectra and the presence of several example, MDP, as bond promoters
groups presented mainly cohesive failures grooves and dispersed silica particles between Y-TZP ceramics and resin-
after 24 hours of water storage, the fail- (seen in Fig. 3C) are representative of based cements, the present investiga-
ures that occurred after 6 months of ag- these ceramic surface modifications. tion reinforces the importance of
ing in water were totally adhesive. This These structural alterations can creating a microretentive and high en-
behavior clearly shows that, irrespective improve the micromechanical inter- ergy surface to enhance and stabilize
of surface treatments, the methacrylated locking between dental ceramics and the bond between them.
phosphoric acid ester present in the resin cements.25,33,38 The same effect
UCem resin cement was capable of pro- was not observed with UCem. The
ducing some type of chemical bonding findings of Mirmohammadi et al21 REFERENCES
with the Y-TZP surfaces. This adhesive could provide an explanation. They 1. Blatz MB. Long-term clinical success of all-
polymeric structure, however, was not showed that, although UCem presented ceramic posterior restorations. Quintessence
strong enough to resist the hydrolytic ef- a good initial bond strength (after Int 2002;33:415-26.
2. Blatz MB, Sadan A, Kern M. Resin-ceramic
fect of water over time.15,30 24 hours) to a Y-TZPebased ceramic bonding: a review of the literature. J Prosthet
Some previous studies showed that (Procera zirconia; NobelBiocare), failure Dent 2003;89:268-74.
airborne-particle abrasion with alumina mode analysis showed predominantly 3. Blatz MB, Richter C, Sadan A, Chiche GJ.
Critical appraisal. Resin bond to dental ce-
particles plus applying MDP is one of interfacial failures. The researchers ramics, Part II: high-strength ceramics.
the most efficient protocols for in- linked these findings to the poor wetta- J Esthet Restor Dent 2004;16:324-8.
creasing the bonding between Y-TZP bility of UCem because of its high vis- 4. Radovic I, Monticelli F, Goracci C,
ceramics and resin cements.12,41 In cosity at the time of application. Thus, it Vulicevic ZR, Ferrari M. Self-adhesive resin
cements: a literature review. J Adhes Dent
contrast, recent studies also showed is reasonable to claim that the same 2008;10:251-8.
that this surface treatment (airborne- phenomenon took place here. In other 5. Zhang C, Degrange M. Shear bond
particle abrasion) may cause micro- words, the sum of the inherent hydro- strengths of self-adhesive luting resins
fixing dentine to different restorative
cracks and induce phase transformation lytic effect of the water and the reduc- materials. J Biomater Sci Polym Ed 2010;21:
in Y-TZP ceramics, potentially triggering tion of the interaction between Y-TZP 593-608.
a decrease in the mechanical properties surfaces and UCem produced by its high 6. Vrochari AD, Eliades G, Hellwig E, Wrbas KT.
Water sorption and solubility of four self-
of the material.42-45 This was the reason, viscosity may have overcome the power
etching, self-adhesive resin luting agents.
in the present study, for testing the of the chemical bonds promoted by the J Adhes Dent 2010;12:39-43.
efficiency of MDP in ceramic surfaces methacrylated phosphoric acid ester 7. Phark JH, Duarte S Jr, Blatz M, Sadan A. An
in vitro evaluation of the long-term resin
without airborne-particle abrasion. This may have prevented UCem from
bond to a new densely sintered high-purity
Testing whether a way to establish a maintaining the bond to Y-TZP surfaces zirconium-oxide ceramic surface. J Prosthet
reliable bond strength to Y-TZP ceramics over 6 months of aging in water.6,8,23 Dent 2009;101:29-38.
exists without additional airborne- This possibility should be investigated. 8. Liu Q, Meng X, Yoshida K, Luo X. Bond
degradation behavior of self-adhesive cement
particle abrasion seemed relevant. and conventional resin cements bonded to
For both resin cements, ceramic silanized ceramic. J Prosthet Dent 2011;105:
CONCLUSIONS 177-84.
surface treatment with MDP-based
9. Manicone PF, Rossi Iommetti P, Raffaelli L.
primer was not capable of maintain- An overview of zirconia ceramics: basic
Within the limitations of the present
ing bond stability over 6 months of properties and clinical applications. J Dent
study, the following conclusions can be
aging in water. This behavior has been 2007;35:819-26.
drawn: 10. Pittayachawan P, McDonald A, Petrie A,
supported by previous studies25,38 and
Knowles JC. The biaxial flexural strength and
may be explained by the poor hydrolytic 1. Irrespective of surface treatments, fatigue property of Lava Y-TZP dental
stability of MDP-based primer. By self-adhesive resin cement was not able ceramic. Dent Mater 2007;23:1018-29.

The Journal of Prosthetic Dentistry da Silva et al

September 2014 575
11. Guazzato M, Albakry M, Ringer SP, 24. Chen L, Shen H, Suh BI. Effect of incorpo- 37. de Sá Barbosa WF, Aguiar TR,
Swain MV. Strength, fracture toughness rating BisGMA resin on the bonding proper- Francescantonio MD, Cavalcanti AN, de
and microstructure of a selection of ties of silane and zirconia primers. J Prosthet Oliveira MT, Giannini M. Effect of water
all-ceramic materials. Part II. Zirconia-based Dent 2013;110:402-7. storage on bond strength of self-adhesive
dental ceramics. Dent Mater 2004;20: 25. Yun JY, Ha SR, Lee JB, Kim SH. Effect resin cements to zirconium oxide ceramic.
449-56. of sandblasting and various metal primers J Adhes Dent 2013;15:145-50.
12. Kern M. Resin bonding to oxide ceramics for on the shear bond strength of resin cement to 38. May LG, Passos SP, Capelli DB, Ozcan M,
dental restorations. J Adhes Sci Technol Y-TZP ceramic. Dent Mater 2010;26:650-8. Bottino MA, Valandro LF. Effect of silica
2009;23:1097-111. 26. Kern M, Barloi A, Yang B. Surface coating combined to a MDP-based primer
13. Thompson JY, Stoner BR, Piascik JR, Smith R. conditioning influences zirconia ceramic on the resin bond to Y-TZP ceramic.
Adhesion/cementation to zirconia and other bonding. J Dent Res 2009;88:817-22. J Biomed Mater Res B Appl Biomater
non-silicate ceramics: where are we now? 27. Song JY, Park SW, Lee K, Yun KD, Lim HP. 2010;95:69-74.
Dent Mater 2011;27:71-82. Fracture strength and microstructure of 39. Wegner SM, Gerdes W, Kern M.
14. Miragaya L, Maia LC, Sabrosa CE, De Y-TZP zirconia after different surface Effect of different artificial aging
Goes MF. Da Silva EM. Evaluation of Self- treatments. J Prosthet Dent 2013;110: conditions on ceramic/composite
adhesive resin cement bond strength to 274-80. bond strength. Int J Prosthodont 2002;15:
yttria-stabilized zirconia ceramic (Y-TZP) us- 28. Aboushelib MN. Evaluation of zirconia/resin 267-72.
ing four surface treatments. J Adhes Dent bond strength and interface quality using a 40. Morresi AL, D’Amario M, Capogreco M,
2011;13:473-80. new technique. J Adhes Dent 2011;13: Gatto R, Marzo G, D’Arcangelo C, et al.
15. Attia A. Bond strength of three luting agents 255-60. Thermal cycling for restorative materials:
to zirconia ceramic: influence of surface 29. Valverde GB, Coelho PG, Janal MN, does a standardized protocol exist in
treatment and thermocycling. J Appl Oral Sci Lorenzoni FC, Carvalho RM, Thompson VP, laboratory testing? A literature review.
2011;19:388-95. et al. Surface characterisation and bonding J Mech Behav Biomed Mater 2013;29:
16. Della Bona A, Borba M, Benetti P, of Y-TZP following non-thermal plasma 295-308.
Cecchetti D. Effect of surface treatments on treatment. J Dent 2013;41:51-9. 41. Kern M, Wegner SM. Bonding to zirconia
the bond strength of a zirconia-reinforced 30. Aboushelib MN, Mirmohamadi H, ceramic: adhesion methods and their dura-
ceramic to composite resin. Braz Oral Res Matinlinna JP, Kukk E, Ounsi HF, Salameh Z. bility. Dent Mater 1998;14:64-71.
2007;21:10-5. Innovations in bonding to zirconia-based 42. Amaral M, Valandro LF, Bottino MA,
17. Baldissara P, Quertzè M, Monaco C, materials. Part II: focusing on chemical Souza RO. Low-temperature degradation of
Scotti R, Fonseca RG. Efficacy of surface interactions. Dent Mater 2009;25:989-93. a Y-TZP ceramic after surface treatments.
treatments on the bond strength of resin 31. Sasse M, Eschbach S, Kern M. Randomized J Biomed Mater Res B Appl Biomater
cements to two brands of zirconia ceramic. clinical trial on single retainer all-ceramic 2013;101:1387-92.
J Adhes Dent 2013;15:259-67. resin-bonded fixed partial dentures: influence 43. Sato H, Yamada K, Pezzotti G, Nawa M,
18. Castro HL, Corazza PH, Paes-Júnior TA, of the bonding system after up to 55 months. Ban S. Mechanical properties of dental zir-
Della Bona A. Influence of Y-TZP ceramic J Dent 2012;40:783-6. conia ceramics changed with sandblasting
treatment and different resin cements on 32. Blatz MB, Phark JH, Ozer F, Mante FK, Saleh N, and heat treatment. Dent Mater J 2008;27:
bond strength to dentin. Dent Mater Bergler M, et al. In vitro comparative bond 408-14.
2012;28:1191-7. strength of contemporary self-adhesive resin 44. Zhang Y, Lawn BR, Rekow ED,
19. Yang B, Barloi A, Kern M. Influence of air- cements to zirconium oxide ceramic with and Thompson VP. Effect of sandblasting on the
abrasion on zirconia ceramic bonding using without air-particle abrasion. Clin Oral Investig long-term performance of dental ceramics.
an adhesive composite resin. Dent Mater 2010;14:187-92. J Biomed Mater Res B Appl Biomater
2010;26:44-50. 33. Wolfart M, Lehmann F, Wolfart S, Kern M. 2004;71:381-6.
20. Matinlinna JP, Heikkinen T, Ozcan M, Durability of the resin bond strength to zirco- 45. Cattani Lorente M, Scherrer SS, Richard J,
Lassila LV, Vallittu PK. Evaluation of resin nia ceramic after using different surface con- Demellayer R, Amez-Droz M, Wiskott HW.
adhesion to zirconia ceramic using some ditioning methods. Dent Mater 2007;23: Surface roughness and EDS characterization
organosilanes. Dent Mater 2006;22: 45-50. of a Y-TZP dental ceramic treated with
824-31. 34. Oyague RC, Monticelli F, Toledano M, the CoJet
Sand. Dent Mater 2010;26:
21. Mirmohammadi H, Aboushelib MN, Osorio E, Ferrari M, Osorio R. Effect of water 1035-42.
Salameh Z, Feilzer AJ, Kleverlaan CJ. aging on microtensile bond strength of dual-
Innovations in bonding to zirconia based cured resin cements to pre-treated sintered
ceramics: part III. Phosphate monomer zirconium-oxide ceramics. Dent Mater Corresponding author:
resin cements. Dent Mater 2010;26: 2009;25:392-9. Dr Eduardo M. da Silva
786-92. 35. de Souza GM, Silva NR, Paulillo LA, De School of Dentistry
22. Piascik JR, Swift EJ, Braswell K, Stoner BR. Goes MF, Rekow ED, Thompson VP. Bond Federal University of Rio de Janeiro
Surface fluorination of zirconia: strength to high-crystalline content zirconia Rua Mário Santos Braga, 30 - Campus Valonguinho
adhesive bond strength comparison to after different surface treatments. J Biomed Centro - Niterói, RJ, 24020-140
commercial primers. Dent Mater 2012;28: Mater Res B Appl Biomater 2010;93:318-23. BRAZIL
604-8. 36. Luthy H, Loeffel O, Hammerle CH. Effect of E-mail: [email protected]
23. Lehmann F, Kern M. Durability of resin thermocycling on bond strength of luting
bonding to zirconia ceramic using different cements to zirconia ceramic. Dent Mater Copyright ª 2014 by the Editorial Council for
primers. J Adhes Dent 2009;11:479-83. 2006;22:195-200. The Journal of Prosthetic Dentistry.

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