Bond Strength of Luting Cements Per Dérand, LDSa

to Zirconium Oxide Ceramics Tore Dérand, LDS, Odont Drb

Purpose: This study was conducted to determine the bond strength of some resin luting
cements to zirconia ceramic. The hypothesis was that adhesive bonding capacity is
influenced by different surface pretreatments designed for milled ceramic inlays.
Materials and Methods: Composite cylinders 5 mm 3 5 mm were light cured on the
ceramic surfaces for a shear test conducted in a test jig. Five surface treatments were
studied: as received (from the milling machine), sandblasting with either 250- or 50-µm
alumina sand, hydrofluoric acid treatment, and grinding with diamond burs. The tested
luting cements were Panavia 21, Twinlook, and Superbond C&B. Results: All debonding
occurred at the interface between ceramic and composite cement. Superbond
demonstrated the highest bond strength regardless of the surface treatments. Grinding the
surface with diamond burs improved the bonding slightly for Twinlook and Panavia 21
and also showed the roughest texture. Washing with hydrofluoric acid had no significant
influence on bond strength. Conclusion: Bond strengths for Twinlook and Pananvia 21
were quite low, and only Superbond showed a bond strength reasonably acceptable for
clinical use; however, as no standard for bond strength has been established for inlay
therapy, the other cements cannot be rejected as luting cements for inlays. Int J
Prosthodont 2000;13:131–135.

C ontemporary ceramic materials provide long-

term service and have excellent esthetic proper-
ties. The decreasing use of dental amalgams prompts
interest in using ceramic inlays. Ceramic inlays can
be fabricated in many ways and in different materi-
als, but computer-aided design and manufacturing
(CAD/CAM) has become an increasingly interesting
alternative to manual, casting, or pressing techniques.
The best-known system is Cerec (Siemens), which has
been in use for a decade.1 Clinical studies have re-
ported good results and a low number of failures.2,3
Although low failure rates are desirable, ditching and
varied marginal adaptation quality seem to be com-
mon problems.4
aPublicDental Service, Norberg, Sweden.
bProfessor,
Department of Oral Technology, Faculty of Odontol-
ogy, Malmö University, Malmö, Sweden.
Reprint requests: Dr Per Dérand, Folktandvården, S-738 30
Norberg, Sweden. e-mail: per.derand@sala.mail.telia.com
A new way to fabricate inlays was recently intro-
duced on the market: Denzir (Dentronic), which uses
zirconia as the ceramic material. The method com-
prises laser light scanning of a working die from an
impression and thereafter milling the inlay. Zirconia
is a high-strength ceramic, about 6 times stronger than
feldspathic porcelains, and it is used as an orthope-
dic material.5 The zirconia material contains Y2O3 as
an additive (3.5 to 6 wt%) to stabilize the ceramic in
a tetragonal phase that is normally not stable at room
temperature. Stresses at crack propagation induce
the transformation of the metastable tetragonal grains
into monoclinic ones that are larger and counteract
further crack propagation. Advantages of this ma-
terial include its strength and ability to be milled in
fine detail. Disadvantages include its quite opaque
appearance.
Most ceramic inlays are adhesively luted to the pre-
pared tooth, and a great number of resin cements have
been introduced on the market.6 Their advantages

Volume 13, Number 2, 2000 131 The International Journal of Prosthodontics

 Bond Strength of Luting Cements to Zirconia
Table 1 Resin Luting Agents Used
Product Components
Rocatec Rocatec Pre
Rocatec Plus
Espesil
Panavia 21 Base
Catalyst
Twinlook Base
Catalyst
Superbond C&B Base
Catalyst
Charisma Minifilled composite
Load
Ceramic
Fig 1 Composite cylinder bonded to the zirconium surface
and fixed in a jig for the shear test.
compared to conventional zinc phosphate cements are
low solubility, good esthetic properties, and the fact
that the adhesion increases the functional strength of
inlays.7 Adhesion of composite to porcelain surfaces
has been widely examined. Etching the inner surface
of a crown or inlay with hydrofluoric acid followed by
the application of a silane varnish is a recommended
method.8–12 The manufacturer recommends Denzir in-
lays to be cemented with conventional cements and
thus mechanically attached to the tooth. The difficulty
in achieving adhesive retention to a zirconia surface
is the main reason for this recommendation.
The aim of this investigation was to examine and
measure the shear bond strength of some resin cements
on zirconia surfaces after different pretreatments.
Materials and Methods
Zirconium oxide ceramic specimens (10 mm 3 5 mm
3 2.5 mm) were milled from ceramic blocks with the
Denzir milling machine. The surfaces were treated
in different ways (Table 1). The 5 groups were cate-
The International Journal of Prosthodontics
Dérand/Dérand
Description Manufacturer
Al2O3 ESPE
Special powder
Silane
Autocuring cement Kuraray
Autocuring cement Kulzer
Autocuring cement Sun Medical
Light-curing composite Kulzer
gorized into (1) as received (cut with a diamond
disk and subsequently treated with Rocatec), (2) air
abraded with 250-µm alumina powder, (3) air
abraded with 50-µm alumina, (4) air abraded with
50-µm alumina powder and etched in 38% hydro-
fluoric acid for 12 minutes, and (5) ground with a
rough diamond bur. The ceramic surfaces were
washed once with silane (Espesil, ESPE), which was
allowed to dry for 10 minutes. Various cements
(Table 1) were then applied and covered with a
mylar film. The cements were allowed to harden for
10 minutes, and composite (Charisma) cylinders
were built up (5-mm diameter and 5-mm height) in
a metallic mold. Altogether, 165 cylinders were
made and the materials were light activated in 2
steps, first for 40 seconds and then for 20 seconds
after removal of the mold (Optilux, Demetron).
One hundred twenty test pieces were kept at 35°C
for 1 to 5 hours (dry) before the shear bond test; sixty-
five pieces from group 5 were divided into three
groups and placed for 1 day, 1 week, or 2 months in
a beaker of tap water (35°C) before the shear test. To
secure the ceramic blocks in a rigid position during
the shear test, they were placed in a brass holder, and
the bond strength was determined in a universal test-
ing device (Alveteron, Lorentz and Wettre). The
crosshead speed was 0.5 mm/min (Fig 1). Failure
mode was examined and classified as adhesive or co-
hesive. The surfaces were inspected with a scanning
electron microscope (SEM), and micrographs were
taken. The results were analyzed with two-way analy-
sis of variance (ANOVA) and the Newman-Keuls test
at a significance level of P < 0.05.
Results
All debonding occurred at the interface between the
ceramic surface and resin cement. Overall, it was ap-
parent that Superbond possessed higher mean bond
strength (! 20 MPa; P < 0.05) than the others, re-
gardless of the surface treatment of the ceramic blocks
(Tables 2 and 3).
132 Volume 13, Number 2, 2000
 Dérand/Dérand Bond Strength of Luting Cements to Zirconia

Fig 2a SEM view of zirconium surface after sandblasting with Fig 2b SEM view of zirconium surface after grinding with a di-
50-µm sand. amond bur.

Table 2 Shear Bond Strengths (MPa) of Composite

Surface treatment with Rocatec resulted in higher Cements on Zirconium Oxide Ceramic (Group 1)
bond strengths for Panavia and Twinlook (Table 3).
Of these, the latter exhibited the weakest bond. Standard
Cement Mean deviation
Grinding the ceramic surface with a diamond bur re-
sulted in a rougher surface than the other treatments Panavia 21 8.9 1.1
Twinlook 8.9 1.0
and, consequently, also in slightly higher bonding Superbond 19.5 2.1
strength (Fig 2). Acid etching of the surfaces with hy-
drofluoric acid demonstrated a weak tendency to
improve bond strength, but the increase was only sig-
nificant for Superbond. Table 3 Shear Bond Strengths (MPa) of Composite
The shear test for specimens stored for 1 week in Cements on Zirconium Oxide Ceramic (Groups 2 to 5)
water showed that the bond strength increased by up
Material Standard
to 20% (Fig 3). After 2 months the values were re- (group) Mean deviation Significance
duced for Panavia 21 and Twinlook but increased
somewhat for Superbond. Superbond (5) 20.1 1.7 s
Superbond (4) 19.9 1.8 t
Superbond (2) 17.7 1.6 s
Discussion Superbond (3) 17.7 1.6 t
Panavia (2) 7.3 1.0 s
Panavia (5) 6.9 0.8 s
An excellent marginal adaptation and a permanent
t
Panavia (3) 5.9 1.5 t s
bond between enamel and ceramic inlays prevent Panavia (4) 5.3 0.8 t

marginal leakage and increase fracture resistance of Twinlook (4) 3.6 0.8 s
Twinlook (5) 3.5 0.7
the inlay. Together with a strong ceramic, inlays offer Twinlook (3) 2.8 1.4
minimized tooth preparation and long-term clinical Twinlook (2) 2.3 0.5 t

service. The bonding of composite to dental porce-
lains has been examined in several respects. Etching
porcelain surfaces with hydrofluoric acid is well
known as a method to increase bond strength.10,13,14
High-strength ceramics like In-Ceram (Vita) and
Procera AllCeram (Nobel Biocare) with dense alu-
minum oxide cores offer no improved bond com-
pared to feldspathic porcelains after etching.15,16
Together with etching, silane treatment improves
bonding of composites to conventional feldspathic
porcelains.17–21 Several products containing silane
compounds are available on the market.
In this study, a high-density zirconia was examined
and the shear bond strength was measured. The milled
Vertical bars indicate no significance (P > 0.05).
surface exposed a moderately rough surface primarily
treated with Rocatec, which implies silica blasting.
Three different resin cements were used, and the re-
sults showed that one (Superbond) was superior to the
others. This resin contains no filler, in contrast to the
other two materials used,22 but all three have demon-
strated good bonding properties.12,21,23 Superbond
contains 4-META/MMA-TBB resin, which is a
crosslinked and very strong adhesive used in several
industrial products. This agent created a bond that
was almost the same regardless of whether the ceramic

Volume 13, Number 2, 2000 133 The International Journal of Prosthodontics

 Bond Strength of Luting Cements to Zirconia
40
30
Bond strength (MPa)
1d
1 wk
2 mo
20
10
0
Panavia 21
Fig 3 Bond strength on surfaces ground with a diamond bur and treated with silane after dif-
ferent times.
surface was etched, sandblasted, or ground. Panavia
and Twinlook had a stronger bond if the ceramic sur-
face was primarily coated with Rocatec. Overall, sur-
face smoothness did not seem to influence bonding,
and mechanical retention was insufficient. The bond
strength was quite low for Panavia and Twinlook and
may be considered too low to ensure good clinical ser-
vice, as a value of around 13 MPa is suggested as the
minimum for acceptable clinical bonding.10 That value
is, however, not applicable to retention of inlays.
The use of hydrofluoric acid gave no improvement
of retention of resin cements. It was not assumed
that it should improve microretention, but rather that
it might possibly change the adhesive capacity of
the ceramic surface or change its potential of free en-
ergy. The results were in accordance with those from
reports where high-density core materials like In-
Ceram and Procera were examined.16,24 Silane cou-
pling agents form very weak or no stable bonds to ce-
ramics with no silica, but may possibly act as weak
wetting agents for resin cements.
Storage in water for 1 week increased the bond
strength, but this improvement was reduced after 2
months for Panavia 21 and Twinlook, a finding that
has been shown in other studies.10,25 One study
showed lower bond strengths after 1 year, but they
varied among surface treatments and materials.26
Use of thermocycling also influences long-term be-
havior to some extent. The influence of water storage
and the extended time need further investigation to
The International Journal of Prosthodontics
Dérand/Dérand
Twinlook Superbond
determine the most important factor, and a long-term
study has been initiated.
The surface roughness was visually different after
grinding with a diamond bur, as the surface exposed
almost parallel ditches. Sandblasting resulted in more
irregular unevenness, but the bond strengths were
only slightly different between the surface treatments.
The results of this study showed that bond strengths
for Twinlook and Panavia 21 were quite low, and only
Superbond showed a bond strength reasonably ac-
ceptable for clinical use; however, as no standard for
bond strength has been established for inlay therapy, the
other cements cannot be rejected as luting cements for
inlays. Surface treatments such as acid etching or sand-
blasting had only minor influence on bond strengths.
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Literature Abstract

Dental considerations in upper airway sleep disorders: A review of the literature.

The purpose of the article was to review the anatomic features and etiologic factors of upper air-
way sleep disorders and current medical and dental options. Approximately 3% of the middle-
aged population suffer from excessive daytime sleepiness that may be the result of frequent
nighttime sleep interruptions caused by upper airway disorders. Upper airway sleep disorders
can have a great negative impact on daily life and cause an increased tendency for accidents.
Children with sleep apnea may exhibit poor school performance and hyperactivity. The estimated
cost to the economy for this disability is billions of dollars! The literature review was conducted
with a literature research tool, PubMed, developed by the United States’s National Library of
Medicine. The etiology of obstructive sleep apnea is apparently multifactorial, and numerous
treatments have been tried. The proper recognition and treatment of these patients are critical
and are mainly a responsibility of the medical profession. After medical evaluation and referral,
dental devices are indicated for snoring and for mild to moderate obstructive sleep apnea pa-
tients. It is now accepted that the dental team can be of help to patients with these disabilities.

Ivanhoe JR, Cibirka RM, Lefebvre CA, Parr GR. J Prosthet Dent 1999;82:685–698. References: 129.
Reprints: Dr John R. Ivanhoe, Department of Oral Rehabilitation, School of Dentistry, Medical College of
Georgia, Augusta, Georgia 30912-1250. e-mail: jivanhoe@mail.mcg.edu—AW

Volume 13, Number 2, 2000 135 The International Journal of Prosthodontics