Dental Materials Journal 2016; 35(1): 29–36

Bonding effectiveness of self-adhesive and conventional-type adhesive

resin cements to CAD/CAM resin blocks. Part 2: Effect of ultrasonic and acid
cleaning
Asuka KAWAGUCHI1*, Mariko MATSUMOTO1*, Mami HIGASHI1*, Jiro MIURA2, Takuya MINAMINO1,
Tomoshige KABETANI1, Fumio TAKESHIGE2, Atsushi MINE1 and Hirofumi YATANI1

1
Department of Fixed Prosthodontics, Osaka University Graduate School of Dentistry, 1-8 Yamadaoka, Suita-shi, Osaka 565-0871, Japan
2
Division for Interdisciplinary Dentistry, Osaka University Dental Hospital, 1-8 Yamadaoka, Suita-shi, Osaka 565-0871, Japan
Corresponding author, Atsushi MINE; E-mail: mine@dent.osaka-u.ac.jp

The present study assessed the effect of ultrasonic and acid cleaning on resin cement bonding to CAD/CAM resin blocks. One of
two resin cements, PANAVIA V5 (PV5) or PANAVIA SA CEMENT HANDMIX (PSA), were bonded to one of 24 CAD/CAM blocks
(KATANA AVENCIA BLOCK). Each cement group was divided into four subgroups: no cleaning (Ctl), ultrasonic cleaning (Uc),
acid cleaning (Ac) and Uc+Ac. Micro-tensile bond strengths (μTBSs) were measured immediately and 1, 3, and 6 months after
water storage. Block surfaces after each treatment were analyzed by scanning electron microscopy. Analysis of variance revealed
a statistically significant effect for the parameters ‘surface treatment’ (p<0.001, F=40), ‘resin cement’ (p<0.001, F=696) and ‘water
aging’ (p<0.001, F=71). The PV5 group exhibited higher μTBS values than the PSA group. Although cleaning after sandblasting was
effective in removing residual alumina particles, it did not affect the long-term bonding durability with non-contaminated CAD/CAM
resin blocks.

Keywords: CAD/CAM, Resin block, Bond strength, Surface treatment, Contamination

indirect) materials6). However, bonding between resin

INTRODUCTION
Computer-aided design/computer-aided manufacturing
(CAD/CAM) technology in dentistry is rapidly
developing to the extent that design and manufacturing
of dental restorations can be carried out either in a
commercial dental laboratory or directly in the dental
office. Compared to conventional methods that rely on
manual work, CAD/CAM technology reduces working
time, improves homogeneity of the restorations and
raises the safety level of the manufacturing process.
This technology was first successfully established for
milling ceramic materials and, today, numerous other
materials have been introduced as a more economical
alternative to dental ceramic restorations1). For example,
composite resin inlays, onlays, veneers and crowns
can be constructed by CAD/CAM techniques using
prefabricated composite resin blocks2) and are claimed
to have the advantages of easier finishing and polishing,
kindness to the natural dentition with regard to wear,
easier add-on adjustment and lower cost compared to
restorations milled from CAD/CAM ceramic blocks3-5).
In addition, restorations from CAD/CAM resin blocks
are naturally more esthetic than those fabricated using
dental alloy.
The standardized polymerization of CAD/CAM resin
blocks under high pressure and temperature yields
significantly better mechanical properties and color
stability compared to conventionally polymerized (direct/
*Authors who contributed equally to this work.
Color figures can be viewed in the online issue, which is avail-
able at J-STAGE.
Received Jul 9, 2015: Accepted Jul 28, 2015
doi:10.4012/dmj.2015-235 JOI JST.JSTAGE/dmj/2015-235
blocks and adhesive resin cements may be challenging
because of the high degree of resin polymerization
established in the blocks. Indeed, Stawarczyk et al.1)
reported that commercially-polymerized CAD/CAM
resin crowns presented significantly lower tensile bond
strengths than those of glass ceramic crowns. Therefore,
in order to establish a sufficient and durable adhesion, it
is crucial to establish the appropriate treatment methods
of the respective surfaces to yield optimal bonding
outcomes7). Our research group recently reported that
sandblasting and silanization significantly increased
micro-tensile bond strength (µTBS) values for bonding
between CAD/CAM resin blocks and adhesive resin
cements8).
In clinical situation, resin block-derived restorations
are vulnerable to fluid contamination such as saliva,
blood or plasma during intra-oral adjustment procedures.
Eiriksson et al.9) reported that saliva contamination
significantly reduced resin-resin bond strengths and
Van Schalkwyk et al.10) reported that during clinical
try-in procedures, contamination of restorative luting
surfaces is difficult to avoid. Therefore, it is important
to ensure the bonding substrate is free of contamination
when bonding is to take place.
The effect of surface contamination with saliva
and subsequent cleaning with phosphoric acid has
been described11,12) and the authors recommend that
restorations be sandblasted to increase bonding
effectiveness. To clean the bonding surface of restoration,
ultrasonic cleaning, which is safe and easy, is frequently
30 Dent Mater J 2016; 35(1): 29–36

used to remove alumina particles that remain on the

resin surface after sandblasting. For these reasons,
manufacturers recommend ultrasonic and acid cleaning
for CAD/CAM resin restorations to clean the surface just
before bonding. These cleaning methods have been used
clinically and some studies reported on the cleaning
effects13,14). However, to date, no study has determined
whether those surface cleaning methods actually
enhance the bonding of adhesive resin cements to the
recently introduced CAD/CAM resin blocks.
The purpose of the present study was to assess
the long-term effect of ultrasonic cleaning and acid
cleaning on CAD/CAM resin blocks as represented
by two outcomes: micro-tensile bond strength (μTBS)
and surface integrity assessed by scanning electron
microscopy (SEM). The hypothesis tested in the present
study was that ultrasonic and/or acid cleaning after
sandblasting improves bonding effectiveness between
CAD/CAM resin blocks and adhesive resin cements.
MATERIALS AND METHODS
Specimen preparation and resin cement build-up
The materials used in the present study are listed in
Table 1 and the experimental procedure is schematically
illustrated in Fig. 1. Twenty four CAD/CAM resin
blocks (KATANA AVENCIA BLOCK, Kuraray Noritake
Dental, Tokyo, Japan), with dimensions 7×7×5 mm,
were randomly divided into 2 adhesive resin cement
groups: PANAVIA V5 group (PV5; Kuraray Noritake
Dental) and PANAVIA SA CEMENT HANDMIX group
(PSA; Kuraray Noritake Dental). The surface of resin
blocks were wet-polished with #400-grit silicon carbide
paper (PRO-ACT, KOHNAN, Osaka, Japan). All blocks
were abraded with 50 μm aluminum-oxide (Al2O3)
particles using a dental airborne-particle abrasion unit
(Adabrader, Morita, Tokyo, Japan) at 0.2 MPa pressure
for 15 s at a distance of 10 mm. Each group was further
divided into 4 subgroups (n=3 blocks per subgroup)

Table 1 Materials, their application procedures and composition

Product
Material (Manufacturer) Composition Application procedure
[Lot number]

KATANA Mixed filler with colloidal silica (Ø40 nm) and aluminum
CAD/CAM AVENCIA BLOCK (Ø20 nm) oxide, Cured resins consisting of methacrylate
—
resin block (Kuraray Noritake) monomer (Copolymer of Urethane dimethacrylate and
[227] other methacrylate monomers), Pigments

Paste A: Bis-GMA, TEGDMA, Hydrophobic aromatic

dimethacrylate, Hydrophilic aliphatic dimethacrylate,
Build up on the
Initiators, Accelerators, Silanated barium glass filler,
PANAVIA V5 (PV5) CAD/CAM resin
Silanated, Fluoroalminosilicate glass filler, Colloidal silica
(Kuraray Noritake) blocks and light-cure
Paste B: Bis-GMA, Hydrophobic aromatic dimethacrylate,
[130926-U] for 20 s for each
Hydrophilic aliphatic dimethacrylate, Silanated barium
2 mm thick.
glass filler, Silanated alminium oxide filler, Accelerators,
Composite dl-Camphorquinone, Pigments
cement Paste A: 10-MDP, Bis-GMA, Triethyleneglycol Dispense equal
dimethacrylate, Hydrophobic aromatic dimethacrylate, amounts of paste A
PANAVIA
Silanated barium glass filler, Silanated colloidal silica, and paste B and mix
SA CEMENT
dl-Camphorquinone, Benzoyl peroxide, Initiators for 10 s. Built up on
HANDMIX (PSA)
Paste B: Bis-GMA, Hydrophobic aromatic dimethacrylate, the CAD/CAM
(Kuraray Noritake)
Hydrophobic aliphatic dimethacrylate, Silanated barium resin blocks and
[1U0049]
glass filler, Silanated colloidal silica, Surface treated light-cure for 20 s for
sodium fluoride, Accelerators, Pigments each 2 mm thick.

Apply on the
K-enchant gel (Et)
CAD/CAM resin blocks
(Kuraray Noritake) Phosphoric acid, water, Colloidal Silica, Dye
for 20 s, rinse for 10 s
[650010]
and air-dry gently.
Others
Clearfil Ceramic Apply on the
Primer Plus CAD/CAM resin
3-trimethoxysilylpropyl methacrylate, MDP, Ethanol
(Kuraray Noritake) blocks for 15 s and
[1F0005] air-dry gently.

Bis-GMA: bisphenol A diglycidyl ether dimethacrylate, TEGDMA: triethyleneglycol dimethacrylate, MDP: 10-methacryloyloxi
decyl phosphoate
 Dent Mater J 2016; 35(1): 29–36 31

Fig. 1 Schematic illustration of the experimental protocol.

1 #400 polishing with a silicon-carbide paper. 2 Each group was further divided into
4 subgroups. All blocks were sandblasted using Adabrader for 15 s. 1: no treatment
(Ctl) subgroup, 2: ultrasonic cleaning (Uc) subgroup, 3: acid cleaning (Ac) subgroup,
and 4: Uc+Ac subgroup. All specimens were silanized after ultrasonic and/or acid
cleaning. 3 Resin cement increments were built up and light cured for 20 s. 4 Each
specimen was stored in 37°C distilled water for 24 h. 5 Each specimen was then cut
into approximately 0.5 mm2 beams. 6 μTBSs of 24 beams per group were measured
immediately after cutting into beams. All remaining beams were stored in water at
37°C. After 1 month, 3 months, and 6 months of water storage, μTBSs per subgroup
were measured. 7 Fractured surfaces after μTBS measurement were analyzed by SEM.

after assignment to one of the following four cleaning
methods:
1. Ctl (control) subgroup: No cleaning treatment.
2. Uc (ultrasonic cleaning) subgroup: Ultrasonically
cleaned for 120 s in distilled water using HI-
SONIC (KS-606N, KYOWA IRIKA, Kanagawa,
Japan) and air dried for 10 s.
3. Ac (acid cleaning) subgroup: Cleaned with 40%
phosphoric acid (K-etchant gel, Kuraray Noritake
Dental) for 20 s, then rinsed with water spray
using a three-way syringe for 10 s and air dried.
4. Uc+Ac (ultrasonic and acid cleaning) subgroup:
Ultrasonically cleaned for 120 s in distilled water,
cleaned with K-etchant gel for 20 s, then rinsed
with water spray using a three-way syringe for 10
s and air dried.
All specimens were silanized for 15 s using Clearfil
Ceramic Primer Plus (Kuraray Noritake Dental) after
ultrasonic and/or acid cleaning and air dried.
Adhesive resin cement (PV5 or PSA) was
incrementally built up on the blocks (2 mm thick for
each layer). Both cements were used following the
manufacturers’ instruction and details of the luting
procedures for each resin cement are presented in Table
1. Each cement layer was light-cured for 20 s with the
same cordless light-emitting-diode curing light (Mini
LED3, SATELEC, Merignac, France) which had a
maximal light density of 2,200 mW/cm2. The blocks were
stored in distilled water for 24 h at 37°C.
Micro-tensile (µTBS) test
The specimens were cut into 32 beams per block with
a slow-speed water-cooled diamond saw (MC-201N,
MARUTO, Tokyo, Japan). The area dimensions of
bonding surface on each beam was approximately 0.7×0.7
mm. The exact dimension of each beam was measured
using a pair of digital calipers. The beams were further
divided into four subgroups for each storage period:
initial (0M) subgroup, 1 month (1M) subgroup, 3 months
(3M) subgroup, and 6 months (6M) subgroup. Of the 96
beams (32 beams×3 blocks), 24 beams were randomly
chosen for initial μTBS group (0M). Remaining beams
were stored in completely sealed bottles containing
distilled water at 37°C for 1, 3 or 6 month (s), and bond
strengths then measured of 24 beams per subgroup. The
water was not changed until measurement. For μTBS
measurement, beams were glued to a jig with Model
repair Ⅱ blue (DENTSPLY-Sankin, Tochigi, Japan) and
tested in a universal testing machine (EZ-test short,
Shimadzu, Kyoto, Japan) at a cross-head speed of 1.0
mm/min until fracture occurred. Means and standard
deviations μTBS were calculated for each subgroup.
SEM evaluation
The block surfaces after each surface treatment
(polishing with #400-grit silicon-carbide paper,
sandblasting, ultrasonic cleaning after sandblasting,
and acid cleaning after sandblasting) (n=4) as well
as the fractured surfaces after μTBS measurement
were analyzed with a scanning electron microscope
(SEM) (JSM-6510LV, JEOL, Tokyo, Japan) to evaluate
morphological differences (Fig. 1). Samples were created
with the same procedure as μTBS test samples. The
fractured surfaces after µTBS test were examined
under SEM to determine the following four failure
modes. Failure modes were classified into 4 groups: [A]
adhesive failure along the cement-block interface; [B]
mixed failure of cement and cement-block interface;
[C] cohesive failure within adhesive resin cement; and
[D] cohesive failure within CAD/CAM resin block. For
SEM observation, samples were mounted with carbon
adhesion tape on a specimen holder and coated with
32 Dent Mater J 2016; 35(1): 29–36

platinum. The SEM was operated at 15 kV.
Statistical analysis
Differences in μTBS values were analyzed using three-
way analysis of variance (ANOVA) and Scheffé’s method
of post-hoc testing. The overall significance level was
set at α=0.05. Statistical software SPSS IBM version
21.0 (SPSS, Chicago, IL, USA) was used for statistical
calculations.
RESULTS
Surface observation
Representative SEM observations of the CAD/CAM resin
block surfaces after each treatment are shown in Fig.
2. The surface after sandblasting was markedly rougher
when compared to the polished surface treated with
#400-grit silicon-carbide paper (Figs. 2a–d). Residual
alumina particles were observed on the block surface in
the Ctl subgroup (Figs. 2c–d). Although particles were
removed by ultrasonic cleaning, small amounts of debris
remained on (Figs. 2e–f). Both alumina particles and
debris were removed by acid cleaning (Figs. 2g–h).
Microtensile (µTBS) test
Mean and standard deviation (SD) of μTBS values
are summarized per group in Table 2 and graphically
presented in Fig. 3. There were no pre-testing failures.
The results of three-way analysis of variance for detected
elements are shown in Table 3. Three-way ANOVA
revealed a significant effect for the parameters ‘surface
treatment’ (p<0.001, F=40), ‘resin cement’ (p<0.001,
F=696) and ‘water aging’ (p<0.001, F=71). Micro-tensile
bond strength values in the PV5 group were significantly
higher than those in the PSA group (p<0.001).
In the PV5 group, μTBS values were significantly
higher in the Ctl subgroup than in Uc (p<0.001), Ac
(p<0.001), and Uc+Ac subgroups (p<0.001). There were
no significant differences in µTBS values between Uc and
Ac subgroups (p=0.84), between Uc and Uc+Ac subgroups
(p=0.94), and between Ac and Uc+Ac subgroups (p=0.99).
In the PSA group, the surface cleaning methods did not
significantly influence μTBS values (p=0.29).
Micro-tensile bond strength values decreased over
time in both PV5 and PSA groups and demonstrated
statistically significant time-dependent differences.
Three-way ANOVA analysis revealed a significant effect
for the parameters: 0M vs. 1M (p<0.001), 0M vs. 3M
(p<0.001), 0M vs. 6M (p<0.001), 1M vs. 3M (p=0.04), 1M
vs. 6M (p<0.001) and 3M vs. 6M (p<0.001).
Failure mode analysis
The fracture mode distribution of PV5 and PSA groups
are shown in Fig. 4 and SEM observations of the
fractured surfaces of the block side are presented in Fig.
5. Regarding the failure mode, cohesive failure within
the adhesive resin cement (failure mode [C], Fig. 5c) was
observed in all test subgroups. Compared to the PV5
group, more specimens exhibited “within cement” failure
in the PSA group. In the PV5 group, 63–92% beams of all
subgroups fractured within the cement, but some beams
showed a mixed failure pattern of cement and cement-
block interface (failure mode [B], Fig. 5b). In the PSA
group, almost all (83–100%) of the beams were broken
within the cement (failure mode [D], Fig. 5d). There was
a morphological difference between the two adhesive

Fig. 2 SEM observation of CAD/CAM resin blocks after surface treatments.

a, b: #400 polishing. Polishing scratches and residual debris on the surface. c, d: Ctl
subgroup. Sandblasting eliminated large debris particles and made the surface rough.
There were some 50 μm size alumina particles on the block surface after sandblasting.
Small debris particles could still be observed under high magnification (arrowheads).
e, f: Uc subgroup. The alumina particles were removed by ultrasonic cleaning. Small
debris particles (arrowheads) remained on the surface. g, h: Ac subgroup. Both alumina
particles and small debris particles after sandblasting were removed by acid cleaning.
Al: alumina particle, Ctl: no cleaning subgroup, Uc: ultrasonic cleaning subgroup, Ac:
acid cleaning group, Uc+Ac: Uc+Ac subgroup.
 Dent Mater J 2016; 35(1): 29–36 33

Table 2 μTBS values (MPa) and type of failure mode

Surface PV5 PSA

treatment 0M 1M 3M 6M 0M 1M 3M 6M

96.5 (10.3) 98.1 (11.5) 89.7 (11.8) 78.0 (14.4) 62.7 (10.4) 60.9 (11.0) 54.0 (10.9) 48.8 (10.0)
Ctl
[4/0/20/0] [2/2/19/1] [4/1/18/1] [3/0/21/0] [0/0/24/0] [0/0/24/0] [0/0/24/0] [3/0/21/0]

87.6 (8.9) 60.0 (9.3) 72.7 (10.4) 64.6 (9.0) 62.6 (9.9) 55.3 (9.4) 55.8 (11.3) 48.8 (10.5)
Uc
[6/2/15/1] [2/0/20/2] [3/0/20/1] [5/0/18/1] [1/0/23/0] [1/0/23/0] [0/0/24/0] [0/0/24/0]

81.1 (7.6) 70.1(11.6) 69.6 (13.9) 70.0 (13.9) 62.6 (9.9) 62.4 (8.2) 49.5 (16.5) 46.1 (14.3)
Ac
[2/1/21/0] [2/0/21/1] [4/0/19/1] [1/0/22/1] [0/0/24/0] [0/0/24/0] [1/2/20/1] [3/0/20/1]

82.9 (11.7) 70.0 (9.8) 70.1 (10.0) 65.9 (14.6) 63.9 (10.9) 62.9 (12.5) 46.7 (10.9) 46.7 (13.1)
Uc+Ac
[4/1/19/0] [4/1/19/0] [2/0/22/0] [3/0/21/0] [0/0/23/1] [1/0/23/0] [0/0/24/0] [2/0/22/0]

Data are shown as means (standard deviation). n=24 per group

Numbers in square brackets are the number of specimens classified into four fracture modes [A/B/C/D]: [A] adhesive failure
along the cement-block interface; [B] mixed failure of cement and cement-block interface; [C] cohesive failure within resin
cement; [D] cohesive failure within CAD/CAM resin block.

Fig. 3 μTBSs in the PV5 group (a) and the PSA group (b).
Outcome of micro-tensile bond strengths (MPa) in the PV5 group (a) and in the PSA
group (b) and outcomes of three-way ANOVA and Scheffé’s method.
Columns connected by a line indicate significant difference (α=0.05). Ctl: no cleaning
subgroup, Uc: ultrasonic cleaning subgroup, Ac: acid cleaning group, Uc+Ac: Uc+Ac
subgroup, 0M: initial, 1M: 1 month water storage, 3M: 3 months water storage, 6M: 6
months water storage.

Table 3 Results of three-way analysis of variance

df Sum of squares Mean square F p

Surface treatment(A) 3 15,235.3 5,078.4 40.025 <0.001

Water aging(B) 3 27,286.65 9,095.5 71.685 <0.001

Resin cement(C) 1 88,432.7 88,432.7 696.965 <0.001

A*B 9 5,828.3 647.6 5.104 <0.001

A*C 3 10,321.6 3,440.5 27.116 <0.001

B*C 3 2,229.7 743.2 5.858 <0.001

A*B*C 9 3,091.4 343.5 2.707 <0.004

Error 736 93,385.6 126.9 — —

34 Dent Mater J 2016; 35(1): 29–36

Fig. 4 The fracture mode distribution in the PV5 group (a) and in the PSA group (b).
Failure modes were classified into 4 groups: adhesive failure; mixed failure; cohesive
failure within the resin cement; and cohesive failure within the CAD/CAM resin block.
In both groups, failures within CAD/CAM resin blocks were rarely observed. In the PSA
group, most specimens were broken within the cement. Ctl: no cleaning subgroup, Uc:
ultrasonic cleaning subgroup, Ac: acid cleaning group, Uc+Ac: Uc+Ac subgroup, 0M: initial,
1M: 1 month water storage, 3M: 3 months water storage, 6M: 6 months water storage.

resin cements (Figs. 5c–d). Many bubbles were observed

on the fractured surfaces in the PSA group but not in
the PV5 group. Adhesive failure (failure mode [A]) was
only shown in 25% of PV5 group samples and in
less than 12.5% of PSA group samples (Fig. 5a). No
differences were observed in the failure mode between
the different storage periods in all subgroups of both
PV5 and PSA groups.

Fig. 5 SEM observation of the block-side of fractured
surfaces after μTBS test.
a: PV5/Uc/1M subgroup. The block surface was
observed. The failure mode was adhesive failure
along the cement-block surface. Only smooth block
surface was observed. b: PV5/Uc+Ac/3M subgroup.
Resin cement and the block surface were clearly
observed on resin block side, indicating that the
failure mode is mixed failure. c: PV5/Uc+Ac/3M
subgroup. Only cement surface was observed
indicating that the failure mode was cohesive
failure within the resin cement. d: PSA/Uc+Ac/0M
subgroup. The failure mode was cohesive failure
within the resin cement. Many bubbles were
shown in the hand-mixed resin cement (arrows).
RB: CAD/CAM resin block, RC: resin cement.
DISCUSSION
The hypothesis —ultrasonic and/or acid cleaning after
sandblasting had positive effect on bonding effectiveness
between CAD/CAM resin block and adhesive resin
cement— is rejected by the findings of this study.
Different outcomes for each surface cleaning method
was clearly observed with the two adhesive resin
cement groups. In the PV5 group, μTBS values for the
Ctl subgroup were significantly higher than those for
other subgroups and there was no significant difference
between Uc, Ac and Uc+Ac subgroups. On the other
hand, there was no significant difference in μTBS values
between any of the surface cleaning subgroups in the
PSA group. Moreover, μTBS values in the PV5 group
were significantly higher than those in the PSA group.
Three-way ANOVA revealed that ‘resin cement’ had the
strongest effect on the bond strength (F=696), suggesting
that choice of cement is an important factor influencing
bonding effectiveness to CAD/CAM resin block. PV5 is
a conventional-type adhesive resin cement and requires
pre-treatment of tooth structure with a self-etch
adhesive agent. It has been reported that this multistep
application technique is complex and technique sensitive
which may preclude the reliability and predictability of
achieving optimal bonding effectiveness15). Many studies,
 Dent Mater J 2016; 35(1): 29–36
conducted in controlled research settings, have reported
that conventional-type adhesive resin cements yield
significantly higher bond strengths than those attained
by self-adhesive resin cements15,16).
In this study, many alumina particles were observed
on block surfaces after sandblasting, and they were
subsequently removed by ultrasonic cleaning (Fig.
2). However, μTBS values in the Uc subgroup were
significantly lower than those in the Ctl subgroup in
the PV5 group, indicating that ultrasonic cleaning did
not contribute to improving and re-capturing lost bond
strength. The disadvantage of performing ultrasonic
cleaning might be water sorption to the resin block
surface. Although the bonding surface was thoroughly
air-dried after ultrasonic cleaning by inspection, the
water component may not be removed completely in
this short time and its residual presence may have
affected polymerization of the hydrophobic resin cement
and weakened the bonding between adhesive resin
cement and resin block. From these results, as long as
restorations are sandblasted after a try-in procedure
in the clinic, it can be said that there is no need for
ultrasonic cleaning.
In all groups of the present experiment, many
beams fractured within the cement and there were more
mixed failures in the PV5 group than in the PSA group.
A previous study reported that the physical properties
of conventional-type adhesive resin cements under long-
term water storage were better than the properties of
self-adhesive resin cements17).
Manufactures recommend both conventional-type
and self-adhesive resin cements for bonding to CAD/
CAM resin blocks. PSA is a self-adhesive, dual cure,
10-methacryloyloxydecyl dihydrogen phosphate (10-
MDP) containing resin cement. Recently, it is reported
that self-adhesive resin cements might be expected to
show similar mechanical bonding quality as conventional-
type adhesive resin cements15). As no bonding agent
or primer is required, self-adhesive cements can save
time and be less technique sensitivite16). In the present
study, μTBS values in the PSA group were significantly
lower than those in the PV5 group and almost all of
the samples were broken within the cement in the
PSA group. In a μTBS test, the weakest part should
be the part that fractures. In this context, evaluation
of mechanical strengths of the adhesive resin cement
correlates to bond strength18). In general, 10-MDP
containing adhesives have always demonstrated good
bonding performance in laboratory and clinical research
environments19,20). However, Yokokawa et al.21) reported
that the mechanical property of the cement itself was
reduced. 10-MDP appeared hydrolytically unstable in
water and, therefore, self-etch adhesives containing water
are expected to compromise clinical performance22,23). In
addition, PSA needs hand mixing, resulting in bubbles
becoming incorporated into the cement (Fig. 5d). Clearly,
the presence of bubbles compromises the mechanical
properties of the cement.
Contamination is a serious problem that challenges
attainment of optimal bonding in clinical situations.
35
Contaminants such as saliva, blood and plasma may
be present in the oral cavity and several studies have
shown that saliva contamination significantly reduces
cement bond strength24). After saliva contamination,
non-covalent adsorption of salivary proteins occurs on
the surface of restorative materials creating an organic
coating that cannot be removed by rinsing with water25).
An advantage of phosphoric acid cleaning is thought
to be its ability to clean contaminated resin surfaces.
Our study group conducted preliminary experiments
using the same materials as the present study to
examine the effect of saliva contamination on CAD/
CAM resin bonding (unpublished data). The results
were: (1) contamination by artificial saliva decreased
μTBS values between adhesive resin cements and resin
blocks; (2) the decrease in μTBS values was recovered by
acid cleaning the surface before bonding. On the other
hand, acid cleaning may have introduced residual water
that inhibited adhesion because it is necessary to flush
the etching agent with water after the acid cleaning
procedure. It is also possible that residual etching
agent may decrease μTBS values. Ishii et al.11) reported
that cleaning with phosphoric acid was ineffective in
removing saliva contamination as shown by the fact that
the initial bond strength and the bond strength after
thermal cycling were both remarkably low. Stawarczyk
et al.6) also reported that phosphoric acid cleaning was
not proven to affect bond strength. The present study
was an in vitro study and the bonding surface was not
contaminated at all so it must be acknowledged that
these laboratory results may not correlate with the
clinical setting. Further studies with contaminated
surfaces are needed.
In evaluating adhesion, the effectiveness of long-
term water storage should be confirmed20). In the
present, samples were cut into 0.7×0.7 mm beams
and stored in distilled water. This storage method is
harsh to the bonding interface; therefore, it is possible
that 6M subgroup data could be viewed as a method
to investigate long-term durability. In actuality, μTBS
values in all groups decreased after long-term water
storage and demonstrated statistically significant time-
dependent differences. The main reasons are considered
to be a decrease in the mechanical strength of the
adhesive resin cement itself and degradation of the
bonding interface. However, in the present study, SEM
observation revealed no changes in the fracture mode
after long-term water storage. Further, a clear process
of bonding degradation could not be observed in the
present study.
Many CAD/CAM resin blocks have been developed
to date and the nature of each block is variable. The
KATANA AVENCIA blocks used in the present study
are made with a relatively new approach26). Therefore,
findings related to this block may not be valid for resin
blocks produced by other companies and additional
investigations are needed to clarify the external validity
of the present study.
36 Dent Mater J 2016; 35(1): 29–36
CONCLUSION
Within the limitations of this study, it was concluded
that both ultrasonic and acid cleaning after sandblasting
did not enhance the long-term durability or strength of
the bond between non-contaminated CAD/CAM resin
blocks and adhesive resin cements. The results suggest
that as long as restorations are sandblasted after the
try-in procedure in the clinical setting, there is no need
for ultrasonic and acid cleaning after sandblasting with
regard to improving micro-tensile bond strength.
ACKNOWLEDGMENTS
The authors would like to express our gratitude to
Kuraray Noritake Dental for the generous donation of
materials used in this study.
Conflict of interest
The authors declare that they have no conflicts of interest
regarding the products herein investigated.
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