Dental Materials Journal 2012; 31(5): 751–757

Influence of air-abrasion and subsequent heat treatment on bonding between

zirconia framework material and indirect composites
Saiji SHIMOE1, Naomi TANOUE2, Kenta KUSANO1, Masayuki OKAZAKI3 and Takahiro SATODA1

1
Department of Anatomy and Functional Restorations, Division of Oral Health Sciences, Hiroshima University Graduate School of Biomedical
Sciences, 2-3, Kasumi 1-Chome, Minami-ku, Hiroshima 734-8553, Japan
2
Division of General Dentistry, Nagasaki University Hospital, 1-7-1, Sakamoto, Nagasaki 852-8501, Japan
3
Department of Biomaterials Science, Division of Molecular Medical Science, Hiroshima University Graduate School of Biomedical Sciences, 2-3,
Kasumi 1-Chome, Minami-ku, Hiroshima 734-8553, Japan
Corresponding author, Saiji SHIMOE; E-mail: shimoe@hiroshima-u.ac.jp

The purpose of this study was to evaluate the influence of air-abrasion and subsequent heat treatment on the shear bond strength
of the bond between indirect composites and a zirconia material. Four surface preparations were employed; ground flat, then heated
to regenerate the crystal phase (C); air-abraded with alumina for 10 s (S10), for 20 s (S20), and air-abraded for 10 s and heated (H).
Disks were primed with Alloy Primer and bonded either with Estenia or with Gradia composite. XRD analysis suggested that the
monoclinic zirconia content was increased by air-abrasion, and decreased by heating. The surface roughness of S10, S20 and H disks
was similar. Nevertheless, H groups showed lower bond strengths than the S10 and S20 groups both before and after thermal cycling.
Although alumina air-abrasion considerably enhanced bonding between zirconia and indirect composites, subsequent heat treatment
had a negative effect on the durability of bond strength.

Keywords: Zirconia, Indirect composite, Bond strength, Air-abrasion, Heat treatment

containing phosphate as adhesive promoters, and 4)

INTRODUCTION
resin cement containing adhesive phosphate monomer.
Yttrium-stabilized tetragonal zirconia polycrystal Among these four methods, air-abrasion is supposed to
(Y-TZP, i.e., zirconia) has been applied to post and core roughen the zirconia, increasing the bonding area and
systems1,2), implant abutments3) and coping for all- modifying the ceramic surface energy and wettability,
ceramic restorations4), because it has an esthetically thus facilitating the formation of resin-zirconia
appealing color, high flexural strength, long-term micromechanical interlocks7-10). This method is effective
stability and good biocompatibility. On the other hand, not only for improving the bonding strength of luting
conventional dental restorations may be coped with a cements but also in bonding to veneering porcelain11,12).
variety of materials: metals, ceramics, composite resin However, the mechanical stress involved in air-
or a combination of these. For zirconia materials to be abrasion initiates the phase transition from tetragonal
more widely applied as a replacement for metal implants to monoclinic zirconia, subsequently resulting in
in restorative dentistry, it is necessary for them to compressive stress13-16). Therefore, heat treatment after
be bonded not only to ceramics but also to composite air-abrasion is recommended when the zirconia is to be
veneering resins (such as required for a composite veneered to porcelain, but no information is available
veneered zirconia crown). about its influence on bonding between zirconia and
In composite resin veneered prostheses, it is indirect composites. Furthermore, the effects may differ
necessary to establish a consistent and durable bond for different indirect composite materials.
between the veneering material and the zirconia The aim of this study was to investigate the effects
substructure. Komine et al.5) demonstrated that the use of of air-abrasion and subsequent heat treatment of the
an acidic functional monomer containing carboxylic zirconia on the shear bond strengths of bonds between two
anhydride (4-methacryloyloxyethyl trimellitate anhydride), different indirect composites and a zirconia framework
phosphonic acid (6-methacryloxyhexyl phosphonoacetate), material. The tested null-hypotheses for this study were
or phosphate monomer (10-methacryloyloxydecyl that the bond strength varies with air-abrasion and heat
dihydrogen phosphate, MDP) could yield a durable, treatment of the zirconia surfaces and that these effects
strong bond between Estenia C&B indirect composite are influenced by the type of indirect composite.
and Katana zirconia. However, apart from one study
with similar findings6), there is little data on the adhesion MATERIALS AND METHODS
of indirect composite resins to zirconia.
In contrast, many studies on bonding with luting Materials used
cements have been reported recently. These studies have Information on the materials is summarized in Table 1.
focused on the potential benefits of: 1) air-abrasion with The zirconia specimens were milled from zirconia blanks
alumina particles, 2) tribochemical coating, 3) primers (Cercon Base, Dentsply International, York, PA, USA)

Received Mar 19, 2012: Accepted May 18, 2012

doi:10.4012/dmj.2012-077 JOI JST.JSTAGE/dmj/2012-077
752 Dent Mater J 2012; 31(5): 751–757

Table 1 List of materials used and their characteristics

System Batch No. Main compositiona Manufacturer

Zirconia
Dentsply International,
Cercon Base 18001606 ZrO2 (92%), Y2O3 (5%), HfO2 (2%), Al2O3, SiO2 (1%)
York, PA, USA
Indirect composites
Bis-GMA, methacrylic acid ester, quartz powder, Kuraray Medical Inc.,
Estenia C&B OA3 00096B
organic hybrid filler Tokyo, Japan
UTMA, methacrylates, glass powder,
DA3 0062AB
alumina micro filler
Gradia FO 907092 UDMA, silica nano powder GC Corp., Tokyo, Japan

OA3 906032 UDMA, silica nano powder

UDMA, inorganic-organic composite filler,
DA3 911162
silica nano powder, glass powder
Primer
Kuraray Medical Inc.,
Alloy Primer 0345AA VTD, MDP, acetone
Tokyo, Japan

UDMA: urethane dimethacrylate; Bis-GMA: bisphenol-A-glycidyl methacrylate; UTMA: urethane tetramethacrylate;

VTD: 6-(4-vinylbenzyl-n-propyl)amino-1,3,5-triazine-2,4-dithiol, or -2,4-dithione tautomer; MDP: 10-methacryloyloxydecyl
dihydrogen phosphate.
a
According to the information provided by the manufacturers

using a CAD/CAM system (Cercon Smart Ceramics, X-ray diffraction (XRD) analyses
Dentsply International). After firing at 1,350°C for six The degree of transformation induced by air-abrasion
hours, disk-shaped specimens 10 mm in diameter and and heat treatment was determined by measuring the
2.5 mm in thickness were prepared. Two types of high- peak intensity ratios in the XRD patterns of the disk-
strength indirect composite materials (Estenia C&B, shaped specimens (n=5 per group). XRD data were
Kuraray Medical Inc., Tokyo, Japan; and Gradia, GC collected with a θ/2θ diffractometer (XD-D1, Shimadzu,
Corp., Tokyo, Japan) originally designed for metal-based Kyoto, Japan) using Cu-Kα radiation at 30 kV and 30
or free restoration were chosen for testing as layering mA. Diffractograms were obtained from 26° to 36° at
materials. A single-liquid primer containing phosphate a scan speed of 1°/min. The monoclinic peak intensity
monomer (Alloy Primer, Kuraray Medical Inc.) was ratio, Xm, was calculated using the Garvie and Nicholson
selected as the adhesion promoter. method17) as follows:

Surface preparation Im(1̄11)+Im(111)

Xm = (1)
All disk specimens were ground flat with a series of Im(1̄11)+Im(111)+It(101)
silicon-carbide abrasive papers (#80, #240 and #600),
and subsequently heated at 1,200°C for 10 min (Jelenko where It and Im represent the integrated intensity (area
Cerafusion VPF MS-1200, J Morita Corp., Osaka, Japan) under the peaks) of the tetragonal (101) and monoclinic
to regenerate the crystal phase (group C), because (111) and (−111) peaks around 30.2°, 31.5°, and 28.2°,
the crystal phase is transformed to monoclinic system respectively. Monoclinic volume content, Vm, was
by grinding in a way that would not occur in clinical calculated using the method of Toraya et al.18):
practice. Some specimens were further treated by air-
abrasion with 50–70 µm alumina (Hi-Aluminas, Shofu 1.311Xm
Vm = (2)
Inc., Kyoto, Japan) for 10 or 20 s (groups S10 and S20, 1+0.311Xm
respectively), followed by washing with a steam cleaner
for 1 min and air-drying. The supply-side air-pressure Surface roughness measurement
during abrasion was 0.3 MPa and the distance from The surface roughness of specimens prepared by each
the orifice to the zirconia surface was approximately 10 different treatment method was measured as the
mm (Jet Blast III, J Morita Corp.). Some of the S10 air arithmetic mean deviation of the profile (Ra) using a
abraded specimens were placed in a furnace at 500°C, surface roughness tester (Surfcorder SE-3300, Kosaka
heated to 1,200°C at a rate of 50°C/min, and then held Laboratory Ltd., Tokyo, Japan). The measurement
at 1,200°C for 10 min (group H). conditions were: cut-off value 0.8 mm, probe 2 µm,
 Dent Mater J 2012; 31(5): 751–757 753

tracing speed 0.05 mm/s and sampling length 2.5 mm. results of the monoclinic zirconia content derived from
The value for each specimen was obtained by measuring the XRD and the surface roughness values were initially
at three arbitrary points and averaging the values. Three analyzed with the Levene test for the evaluation of
specimens were evaluated for each different treatment equality of variance. The means of each group were also
method. analyzed by one-way ANOVA and Scheffé or Tukey HSD
post hoc pairwise comparison tests (α=0.05).
Shear bond strength (SBS) testing and failure analysis The SBS results were compared with three-way
16 disk-shaped specimens were prepared for each of the analysis of variance (ANOVA) after the Levene test for
four surface preparations (C, S10, S20, H). A piece of the evaluation of equality of variance. Then, for each
double-sided tape with a circular hole 5 mm in diameter thermocycling status, the values of each treatment-
was positioned on the surface of each zirconia specimen indirect composite were compared by one-way ANOVA,
to define the bonding area. Then the Alloy Primer was and post-hoc Scheffé tests were performed with the value
applied to the zirconia surfaces of all 4×16 disks using a of statistical significance set at α=0.05. In addition, to
sponge pellet. analyze the influence of the thermal cycling, the results
A thin layer of one of two opaque resins (Gradia FO, of the samples from an identical surface treatment
GC Corp., or Estenia C&B OA3, Kuraray Medical Inc.) subjected to 0 or 20,000 thermal cycles were compared
was applied to each zirconia surface and exposed to light using Mann-Whitney’s U tests with the value of
for 60 s (Gradia) or 90 s (Estenia C&B) in a polymerizing statistical significance set at α=0.05 for each treatment.
unit (Hi Light power, Heraeus Kulzer GmbH, Wehrheim, All analyses were carried out using IBM SPSS 19.0 (IBM
Germany). An additional opaque material (Gradia OA3, Japan Inc., Tokyo, Japan).
GC Corp., Estenia C&B OA3, Kuraray Medical Inc.)
was applied twice on top of the primary opaque resin, RESULTS
each of which was exposed to light for the same duration
as the first layer. After light-exposure, a brass ring XRD results
(6 mm inside diameter, 2 mm length, and 1 mm wall The XRD patterns after grinding followed by heating
thickness) was placed surrounding the opaque resin. to regenerate the crystal phase (C), air-abrasion for 10
The ring was filled with a dentin shade of the indirect or 20 s (S10 or S20), and heat treatment after abrasion
composite material (Gradia DA3, GC Corp., Estenia for 10 s (H) are shown in Fig. 1. The diffraction peaks
C&B DA3, Kuraray Medical Inc.). All specimens were
then light cured with the polymerization unit for 300 s,
and the Estenia specimens received a further final heat-
polymerization at 110°C for 15 min in an oven (KL-100,
J. Morita Corp.).
Thirty minutes after preparation, the specimens
were immersed in water at 37°C for 24 h, and this state
was defined as thermal cycle 0. Each set of 16 disks was
then divided into two groups of 8 specimens: half (four
sets of 8 specimens) were tested to determine the 24-h
SBS without thermal cycling. The remaining specimens
were placed in a thermal cycling apparatus (Thermal
Cycler, Nissin Seiki Co. Ltd., Hiroshima, Japan) and
cycled between 4°C and 60°C water, with a 1-min dwell
time per bath, for 20,000 cycles.
Prior to SBS testing, the specimens were positioned
in steel molds, and seated in a shear-testing jig. SBS
were determined by means of a mechanical testing
device (AGS-J, Shimadzu, Kyoto, Japan) at a crosshead
speed of 0.5 mm/min. The fractured interfaces were
observed with an optical microscope (×8; S300II, Inoue
Attachment Corp., Tokyo, Japan) and the failure modes
were recorded as either: adhesive failure at the zirconia-
resin interface (A), a combination of cohesive and
adhesive failures (AC), or cohesive failure within the
resin (C). Representative specimens were observed with
a scanning electron microscope (SEM, VE-8800, Keyence
Corp., Osaka, Japan).
Fig. 1 XRD patterns of zirconia after each treatment.
Statistical analysis (C) ground flat; (S10) air-abraded with alumina
For all tests, the mean and standard deviation (SD) for 10 s; (S20) for 20 s; (H) air-abraded for 10 s
for each set of surface treatments was calculated. The and heated.
754 Dent Mater J 2012; 31(5): 751–757

due to monoclinic zirconia increased after both of the S20, H) showed significantly higher Ra values than
air-abrasion treatments (S10 or S20) as compared with the control group (C) (p<0.05). The surface roughness
C group samples, and the peaks for tetragonal zirconia increased with increasing air-abrasion time, with the
decreased conversely. In contrast, the XRD pattern S20 group showing significantly higher Ra than the S10
of H group samples showed an increase in the peaks group (p<0.05). Comparison between samples with or
corresponding to tetragonal zirconia. The peaks of the without heat treatment after air-abrasion for same time
H group samples after heat treatment were nearly (10 s, i.e. the S10 group and the H group) showed that
identical to those of the C group before air-abrasion. there was no significant difference in Ra value (p>0.05).
The monoclinic zirconia contents derived from the
XRD patterns using equations (1) and (2) are shown in SBS and failure results
Table 2. The monoclinic zirconia contents of S10 and S20 Means and standard deviations of SBS in MPa for the
groups were significantly larger than those of the C and different sample groups and percentages of each failure
H groups (p<0.05). There was no significant difference mode are shown in Table 3. The SBS values for both
in monoclinic content between H group and C group indirect composites, with both thermal cycling statuses,
(p>0.05). were significantly higher for the S10 and S20 groups than
the C groups (p<0.05). There was no significant difference
Surface roughness results between S10 and S20 groups (p>0.05). However, the H
The surface roughness values of the zirconia surfaces group showed significantly lower bond strength than
tested are shown in Table 2. Air-abraded groups (S10, S10 and S20 groups (p<0.05). Some differences were
seen with thermal cycling - the strengths of C (Gradia)
and H (Estenia, Gradia) groups at 20,000 thermal
cycles were significantly lower than the corresponding 0
Table 2 Means and standard deviations of monoclinic thermal cycle data (p<0.05). The number of combination
content and surface roughness values (Ra) for adhesive and cohesive failures (AC) was reduced for all
each group groups by application of thermal cycling. All specimens
in the H groups for both indirect composites showed
Monoclinic content Surface roughness
Groups adhesive failure (A) after thermal cycling.
(SD) (vol%) (SD) (μm)
Electron micrographs of representative thermally
C 0.74 (0.15)A 0.05 (0.01)a cycled and debonded composite-zirconia surfaces are
shown in Fig. 2. When Gradia was used after air-
S10 4.61 (1.02)B 0.45 (0.02)b
abrasion (S10, S20 groups), composite residues are
S20 5.44 (0.49)B 0.50 (0.03)c identified on the zirconia surface (Figs. 2f and g).
Complete detachment from the zirconia surface occurred
H 0.99 (0.25)A 0.46 (0.03)b in almost all specimens except for the abovementioned
Within the same column, different letters indicate groups groups (Figs. 2 a–e, and h).
that are statistically different (p<0.05).

Table 3 Means (MPa) and standard deviations of shear bond strengths

0 thermal cycle 20,000 thermal cycles

Composites
Groups Mean (SD) A AC C Mean (SD) A AC C

C 1.1 (0.1) A
100% – – 1.2 (0.4) a
100% – –

S10 13.7 (2.2) C

100% – – 12.4 (3.0) c
100% – –
Estenia
S20 13.6 (2.1) C 75% 25% – 13.9 (3.3) c 87.5% 12.5% –

H 6.3 (0.8) B 87.5% 12.5% – 3.1 (1.8) a,b * 100% - –

C 18.3 (1.0) D
– 100% – 1.4 (0.2) * a
87.5% 12.5% –

S10 24.6 (3.0) E

25% 75% – 22.4 (2.1) d
37.5% 62.5% –
Gradia
S20 23.0 (1.5) E 25% 75% – 21.5 (3.4) d 50% 50% –

H 19.7 (2.0) D 37.5% 62.5% – 6.9 (2.8) b * 100% – –

Within the same column at each composite, mean with the different letters are statistically different (p<0.05), *: significant
difference from 0 thermal cycle bond strength at the same group (p<0.05). A: adhesive; AC: combination of cohesive and
adhesive; C: cohesive.
 Dent Mater J 2012; 31(5): 751–757 755

Fig. 2 Scanning electron micrographs of representative thermally cycled and debonded composite-
zirconia fracture surfaces:
(a) Estenia-C group; (b) Estenia-S10 group; (c) Estenia-S20 group; (d) Estenia-H group; (e)
Gradia-C group; (f) Gradia-S10 group; (g) Gradia-S20 group; (h) Gradia-H group.
756 Dent Mater J 2012; 31(5): 751–757

Thus, it seems that difference in bond strength was

DISCUSSION
affected by these factors.
Air-abrasion of the zirconia surface is an important Regardless of the thermal cycling status, many
treatment method to get a strong bond to veneering groups showed a high percentage of adhesive failures,
porcelain. However, the mechanical stress initiates a and no cohesive failures were seen in any group (Table
phase transition to monoclinic zirconia, and the phase 3, Fig. 2). The result is different from previous studies
transition gives rise to volume expansion and reduction which showed mostly cohesive failures using phosphate
in coefficient of thermal expansion. Therefore, the monomer and resin cement8,10,27). This indicated that
phase transition needs to be reversed to the tetragonal there is a problem at the interface between zirconia
zirconia by heat treatment. In contrast, the effect of heat and the composites, which is likely to be because of the
treatment after air-abrasion on the bonding of indirect physical properties of the composite such as wettability
composites to zirconia is not known. or filler size. In addition, the H group after thermal
In this study, at first, the monoclinic zirconia cycling showed only adhesive failures with both indirect
contents produced by air-abrasion and subsequent heat composites. These results suggest that although the
treatment were determined by calculation from XRD bond strength values vary with the type of indirect
data. The monoclinic zirconia content was increased by composite, the influences of air-abrasion and subsequent
air-abrasion stress (S10 and S20 groups), in accordance heat treatment are not changed.
with air-abrasion time (Table 2). However, the Usually, the transformation from tetragonal to
monoclinic content induced by air-abrasion stress was monoclinic zirconia induced by air-abrasion expands their
largely reversed by heat treatment (H group). These volume to generate compressive stress on the surface,
results were very similar to previous studies16-18). Then, resulting in an increase in strength, and subsequent
the surface roughness resulting from four different regeneration of tetragonal phase by heat treatment
surface preparations (C, S10, S20, H) was examined in reduces the compressive stress on the surface, resulting
terms of Ra (Table 2). The values for the air-abraded in a decrease in strength28). Furthermore, neither of
groups were significantly higher compared with the the coefficients of thermal expansion of tetragonal or
ground flat group, and the roughness also increased monoclinic zirconia is compatible with those of indirect
in accordance with air-abrasion time. However, in this composites19-22). Thus, within the limitations of this
case, the S10 group was not significantly different from study it was possible to conclude that air-abrasion is an
the H group in surface roughness. These two groups effective method to enhance bonding between zirconia
had the same air-abrasion time. This means that the and indirect composites, whereas heat treatment after
surface roughness is not altered by the temperatures air-abrasion is not necessary.
used in our heat treatment15). These results show that
the air-abrasion pressure can increase the monoclinic CONCLUSION
zirconia content with increase of surface roughness.
However, the heat treatment only reverses the increase Within the limitations of this study, it was possible
in monoclinic zirconia content, and does not affect the to conclude that air-abrasion is highly effective in
surface roughness. improving bonding between indirect composite and
The results of the present study show that the bond primed zirconia (Y-TZP). However, heating the zirconia
strengths of samples in the H groups were lower than S10 after air-abrasion decreases the bond strength with the
and S20 groups for both indirect composites regardless indirect composites studied.
of thermal cycling, and that these strengths were also
significantly decreased by thermal cycling (Table 3). As ACKNOWLEDGMENTS
shown above, S10 and S20 groups had higher monoclinic
contents than H group. The coefficient of thermal This work was supported in part by Grants-in-Aid for
expansion of monoclinic zirconia (7.5×10−6/°C)19,20) is Scientific Research (C 20592302 in 2008 and C 21592453
significantly lower than that of tetragonal zirconia (10– in 2010) from the Japan Society for the Promotion of
10.5×10−6/°C)21). However, this cannot be regarded as an Science (JSPS).
influence on strength of bonds to indirect composites,
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