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Article history: Objectives. The purpose of this laboratory study was to evaluate the influence of different
Received 18 April 2005 cleaning methods after saliva contamination and after using a silicone disclosing medium
Received in revised form on the resin bond strength to zirconia ceramic. The hypothesis was that the resin-ceramic
6 March 2006 bond strength and its durability are related to the ceramic surface condition.
Accepted 8 March 2006 Methods. Plexiglas tubes filled with composite resin were bonded to air-abraded zirconia
ceramic disks using a phosphate monomer containing composite resin. Four surface clean-
ing methods were used after contaminating the ceramic surface: air abrasion with 50 m
Keywords: Al2 O3 at 2.5 bar pressure for 15 s, cleaning with 37% phosphoric acid for 60 s once or for 30 s
Bond strength twice, or cleaning in 96% isopropanol for 15 s. The specimens of the control group were not
Cleaning methods cleaned after using the silicone disclosing medium. For each combination 16 specimens
Cercon were bonded in an alignment apparatus. Subgroups of eight bonded specimens were tested
Air abrasion for tensile bond strength (TBS) after storage for either 3 or 150 days combined with 37,500
Zirconia ceramic thermal cycles. The statistical analyses were performed with the Kruskal–Wallis test, fol-
Panavia F 2.0 lowed by multiple pair-wise comparisons using the Wilcoxon rank sum test.
Silicone disclosing medium Results. The mean TBS ranged from 6.6 to 49.9 MPa after 3 days and from 0 to 19.8 MPa after
Fit checker 150 days. Air abrasion of the ceramic surface provided statistically significantly higher bond
strengths than the other cleaning methods after 3 and 150 days. Alcohol cleaning of the
ceramic did not provide durable bond strengths over time.
Significance. Ceramic cleaning methods after try-in procedures have a significant influence
on the resin-ceramic bond strength. Air abrasion of contaminated zirconia ceramic is the
most effective.
© 2006 Published by Elsevier Ltd on behalf of Academy of Dental Materials. All rights reserved.
∗
Corresponding author. Tel.: +49 431 5972874; fax: +49 431 5972860.
E-mail address: mkern@proth.uni-kiel.de (M. Kern).
0109-5641/$ – see front matter © 2006 Published by Elsevier Ltd on behalf of Academy of Dental Materials. All rights reserved.
doi:10.1016/j.dental.2006.03.008
d e n t a l m a t e r i a l s 2 3 ( 2 0 0 7 ) 506–512 507
clinical situations, such as compromised retention and short methods after saliva contamination and after using a silicone
abutment teeth [9] or for resin bonded FPDs [4,5,10]. High- disclosing medium on the resin-ceramic bond strength of an
strength ceramic materials such as zirconium oxide-based adhesive bonding system to zirconia ceramic. The study was
ceramics require alternative bonding techniques to achieve a designed to test the hypothesis that the resin-ceramic bond
long-term durable resin-ceramic bond because conventional strength and its durability are related to the cleaning meth-
hydrofluoric etching has no positive influence on the bond ods of the contaminated ceramic bonding surface.
strength [11]. Compared with silica-based ceramics, in the
literature only a few studies regarding bonding methods to
zirconium oxide ceramics have been published. These studies 2. Materials and methods
suggest the use of resin cements that contain special adhesive
monomers [12–16]. Disk-like specimens were made from the zirconia ceramic Cer-
All-ceramic restorations finished for cementation are usu- con (94% ZrO2 stabilised by 5% Y2 O3 , DeguDent, Germany,
ally already air-abraded from the dental laboratory. After the Batch No. 20009176). The disks had a diameter of 8 mm and
try-in of the restoration again, the ceramic surface might be a thickness of 3.4 mm. All specimens were polished with a
contaminated by saliva, blood or silicone fit-indicators. The rotating silicon carbide paper down to 600 grit and airborne
use of a silicone disclosing medium allows the dentist to particle abraded with 50 m Al2 O3 at 2.5 bar pressure (15 s)
improve the fit of dental restorations by detecting interfer- at a distance of 10 mm at most, 1 h before bonding. After-
ence spots on the internal casting surfaces before cemen- wards, the specimens were immersed in saliva for 1 min.
tation. However, residual organic and silicone contaminants Saliva was collected from the first healthy author who had
may decrease bond strengths and should be removed from refrained from eating and drinking 1.5 h prior to the collec-
the surface before cementation. tion procedure. All experiments were performed using fresh
Saliva contamination of etched enamel is one of the most saliva collected at the same occasion. The specimens were fol-
frequent reasons for poor or failed bond strength. A recent lowed by water-spraying for 15 s and air-drying for another
study evaluated the effects of various saliva contamination 15 s. Then the specimens were pressed into the freshly mixed
periods on the surface topography of etched enamel sur- silicone disclosing medium (Fit Checker black, GC Corporation,
faces [17]. It could be shown that the salivary contaminant Tokyo, Japan) with finger pressure for 3 min. Because there
could be successfully removed by water-rinsing only when were no visible remnants after removing the black silicone
the salivary exposure time is less than 1 s. Salivary exposure fluid, the specimens were not cleaned with water spray. All
times of more than 1 s will lead to an adherent organic coat- specimens were cleaned using the following methods. Then a
ing that is not removed by conventional washing methods phosphate monomer modified composite resin (Panavia F2.0,
and it would be necessary to repeat the etching procedure. Kuraray, Osaka, Japan) was applied to the cleaned ceramic sur-
The effect of ceramic surface contamination with saliva and face. Four different ceramic cleaning methods were used after
the subsequent cleaning of the surface with phosphoric acid contamination and the following codes were assigned to the
was evaluated by Nicholls et al. [18]. Comparing two differ- groups:
ent surface cleaning methods, cleaning with phosphoric acid The specimens were classified into five experimental
showed higher bond strength values than cleaning with ace- groups according to the cleaning methods: air-abraded with
tone. However, the bond strength was evaluated without the 50 m Al2 O3 at 2.5 bar pressure for 15 s at a distance of 10 mm
influence of long-term water storage and long-term thermal and then air cleaned with compressed air (group AIR); etched
cycling so that there is no indication for the bonding durabil- with 37% phosphoric acid for 60 s once, then rinsed with
ity. water spray for 15 s and dried for another 15 s (group PH1);
Szep et al. evaluated the influence of silicone disclosing etched with 37% phosphoric acid for 30 s twice and then water-
procedures on the shear bond strength of composite cements sprayed for 15 s and dried for 15 s (group PH2); immersed in
to industrially sintered (Cerec) and laboratory sintered (Duc- 96% isopropanol for 15 s and then rinsed with tap water for
eram) ceramic restorations after differently conditioning the 15 s (group ALC); or rinsed with tap water only (group CTR).
ceramic surface [19]. This study showed that etching the spec- Table 1 shows the composition of the used materials.
imens with 9.5% hydrofluoric acid (HF) for 60 s after using a Plexiglas tubes with an inner diameter of 3.2 mm were filled
fluid silicone did not lead to a significant reduction of the with auto-curing composite resin (Clearfil FII, Kuraray Med-
shear bond strength between ceramic and composite cement. ical Inc., Osaka, Japan). After 7 min from mixing, the filled
Another study found that the use of a silicone fit-indicator tubes were bonded with Panavia F 2.0 composite resin (Kuraray
significantly reduced the crown retention bonded with zinc Medical Inc., Osaka, Japan) to the ceramic surface using an
phosphate cement because of a residual silicone film remain- alignment apparatus under a load of 750 g [21]. The appa-
ing on the inner surface of the crown [20]. Cleaning with a ratus ensured that the tube axis was perpendicular to the
metal cleaner before cementation did not reverse the effect. surface (Fig. 1). After excess resin was removed, an air block-
Therefore, after the try-in of restorations in a patient’s mouth, ing gel (Oxyguard II, Kuraray Medical Inc., Osaka, Japan) was
they should be air-abraded with Al2 O3 before cementation. In applied around the bonding margins. The bonded specimens
short, after using a silicone disclosing medium, silicone rem- were light-cured for 20 s from two opposite sides with a den-
nants may decrease bond strengths and should be removed tal curing light machine (Optilux 500, Kerr, Danbury, USA),
from the surface before bonding. further cured in a light-curing unit (UniXS, Heraeus-Kulzer,
Therefore, the purpose of this laboratory study was to Wehrheim, Germany) for an additional 90 s, and placed at
evaluate the influence of different ceramic surface cleaning room temperature for 10 min, and then stored in 37 ◦ C water.
508 d e n t a l m a t e r i a l s 2 3 ( 2 0 0 7 ) 506–512
Cercon Base 38 20009176 ZrO2 (94%),Y2 O3 (5%), Al2 O3 (<1%),Si2 O3 (<1%) cont. ceramic DeguDent, Hanau, Germany
Fit Checker Base paste 0301161 Si cont. silicone GC Corporation, Tokyo, Japan
Black Catalyst paste 0301161 Sn cont. silicone
BisGMA, bisphenol-A-diglycidylmethacrylate; BPEDMA, bisphenol-A-polyethoxy dimethacrylate; DMA, aliphatic dimethacrylate; MDP, 10-
methacryloyloxy-decyl dihydrogenphosphate; TEGDMA = triethyleneglycol dimethacrylate, Al, aluminum; B, boron; Ba, barium; Si, silicium;
Sn, stannous; Zr, zirconium; Y, yttrium; cont., containing.
a
According to the information provided by the manufacturers.
Fig. 1 – Test configuration. Alignment apparatus (left), thermal cycling apparatus (middle), and self-aligning debonding jig
with upper and lower rings for chain suspension (right).
d e n t a l m a t e r i a l s 2 3 ( 2 0 0 7 ) 506–512 509
AIR, air-abraded with 50 m Al2 O3 at 2.5 bar pressure (15 s); PH1,
cleaned with 37% phosphoric acid for 60 s; PH2, cleaned with 37%
Fig. 2 – Type of bonding failure mode as identified with a
phosphoric acid twice for each 30 s; ALC, cleaned in isopropanol
(96%); CTR, control group without cleaning. Storage time 3 days light microscope at 30× magnification and calculated in
was without thermal cycling, while storage time 150 days included percentage of the bonding area for all test methods after
37,000 thermal cycles. Within the same column, means with the different storage times. Group codes see Table 2.
same letter are not statistically different (p > 0.05). Within the same
row, means with the same Greek letter are not statistically different
p > 0.05. Global Kruskal–Wallis test followed by pair-wise compari-
son using the Wilcoxon test.
In groups ALC and CTC the failure modes were completely
adhesive for all specimens after 3 days and 150 days storage
time.
ranging from 14.7 to 32.2 MPa. It also decreased statistically SEM sample photographs of groups PH1 and PH2 demon-
significantly after storage time (7.4–20.4 MPa). strated a change in failure mode over storage time. After
The specimens cleaned in alcohol (group ALC) showed rel- storage over 150 days with thermal cycling, the failure mode
atively low initial bond strengths from 0 to 15.4 MPa. Three changed to mostly adhesive in group PH1 (about 60%), while
specimens debonded spontaneously during the storage of 3 in groups AIR and PH2 the portion of adhesive failures was
days. lower (about 25–50%). Figs. 3–5 show representative SEM pho-
No cleaning after contamination (group CTR) led to the low- tographs of the debonded ceramic surfaces after tensile test-
est bond strength values, initially ranging from 0 to 18.0 MPa. ing. The examination of typical samples in the SEM verified
After 3 days two specimens debonded spontaneously. During the failure modes detected with the light microscopic evalu-
the next 12 days storage time, all specimens of groups ALC ation (LM) in groups AIR, PH1 and PH2 (Figs. 3 and 4) and in
and CTR debonded spontaneously. Therefore, cleaning with groups ALC and CTR (Fig. 5).
alcohol and no cleaning in the control group resulted in a sta-
tistically significant decrease of bond strength compared to
the other cleaning methods after 3 and 150 days of storage
time, respectively.
Air abrasion of the zirconium oxide specimens with Al2 O3
increased the bond strength statistically significantly, but
it did not remain stable over storage time. Moreover, TBS
of group PH2 is statistically significantly higher than that
of group PH1 after 3 days storage. However, after 150 days
there was no statistically significant difference between TBS
of groups PH1 and PH2. In summary, the long-term stor-
age in water with thermal cycling led to a statistically
significant decrease in tensile bond strength for all test
groups.
The types of failure modes as assigned using the light
microscope at 30× magnification and calculated in percent-
ages of the bonding areas for all groups, are shown in
Fig. 2. Initially after 3 days of water storage the failure
mode was mostly cohesive in the tube filling composite Fig. 3 – Type of failure mode in group AIR after 3 days of
resin for groups AIR, PH1 and PH2. In group PH1 the per- storage time. A, very small part of adhesive failure from
centage of adhesive failure was about three times higher ceramic surface; C1, cohesive failure in Panavia F 2.0
than that in groups AIR and PH2. After 150 days storage composite resin cement; C2, cohesive failure in the tube
the percentage of adhesive failure increased in all groups. resin. SEM: 50× magnification.
510 d e n t a l m a t e r i a l s 2 3 ( 2 0 0 7 ) 506–512
Fig. 4 – (a) Type of failure mode in group PH1 after 150 days of storage time and TC. A, adhesive failure from ceramic
surface; C1, cohesive failure in Panavia F 2.0 composite resin cement; C2, cohesive failure in the tube resin. SEM: 50×
magnification. (b) Detailed magnification of (a) part A. Air-abraded ceramic surface with only minimal coatings, which
points at an adhesive failure mode. SEM: 4000× magnification. (c) Detailed magnification of (a) part C1. Organic matrix could
be seen, which points to a cohesive failure in the composite resin. SEM: 1000× magnification. (d) Detailed magnification of
(a) part C1. There are bubbles seen from mixing the tube resin. SEM: 1000× magnification.
(3) In previous studies high and durable bond strengths [13] Blatz MB, Sadan A, Kern M. Adhesive cementation of
to zirconia ceramic were achieved with the phosphate high-strength ceramic restorations: clinical and laboratory
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methods and their durability. Dent Mater 1998;14:64–71.
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age time. Therefore the clinical use of Panavia F2.0 for zirconia ceramic. J Adhes Dent 2000;2:139–45.
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