Influence of Ambient Air and Different Surface Treatments

on the Bonding Performance of a CAD/CAM Composite

Block
Alghamdi Alia / Tomohiro Takagakib / Toru Nikaidoc / Ahmed Abdoud /Junji Tagamie

Purpose: To evaluate the bond strengths of time elapsed after sandblasting with alumina particles on a CAD/CAM
composite block treated with different surface conditioning methods.
Materials and Methods: A CAD/CAM composite block (CCB) was cut into 72 slices of approximately 2 mm thick-
ness. The CCB slices were divided into three groups according to sandblasting pressure (0.1 MPa, 0.2 MPa, or un-
treated), and then divided into two subgroups according to the time elapsed after sandblasting: same-day or
one-week dry storage under controlled laboratory conditions before cementation. Surface roughness was observed
by confocal laser microscopy (CLSM) (n = 20); then the wettability of the CCB surfaces was examined using a con-
tact angle (CA) measuring device on a droplet of deionized water (n = 12). Next, CCB slices were divided into three
subgroups according to the surface treatment: Clearfil Ceramic Primer (CP), Clearfil Universal Bond (UB), or a mix-
ture of Clearfil Porcelain Bond Activator and Clearfil tri-S Bond ND Quick (NDP). All CCB slices were then cemented
with Panavia V5 and stored at 37°C in distilled water for 24 h and cut into sticks (n = 10). The sticks were sub-
jected to microtensile bond strength (µTBS) testing, and failure mode analysis was performed using scanning elec-
tron microscopy. The µTBS results were subjected to 3-way and 2-way ANOVA (α = 0.05).
Results: All groups showed a statistically significant increase in wettability accompanied by decreased µTBS after
one week; however, the UB group exhibited stable performance after one week.
Conclusion: The time elapsed after sandblasting with alumina particles affects the bond strength, but it had no sig-
nificant effect on the UB group.
Keywords: alumina particles, CAD-CAM, composites, microtensile bond strength, silane, sandblasting, wettability

J Adhes Dent 2018; 20: 317–324. Submitted for publication: 20.06.16; accepted for publication: 09.07.18
doi: 10.3290/j.jad.a40993

a PhD Candidate, Cariology and Operative Dentistry Department, Graduate

School of Medical and Dental Sciences, Tokyo Medical and Dental University,
Tokyo, Japan. Participated in experimental design, performed the experi-
D igitization of dental practice has been progressing glob-
ally, improving the quality of the restorations and time
management, while markedly reducing costs. Computer-
ments, wrote the manuscript.
aided design/computer-aided manufacturing (CAD/CAM)
b Assistant Professor, Cariology and Operative Dentistry Department, Graduate
School of Medical and Dental Sciences, Tokyo Medical and Dental University,
applications in dentistry are expanding rapidly, thanks in
Tokyo, Japan. Idea, hypothesis, experimental design, proofread the manuscript. part to the wide use of silicate and non-silicate ceramics as
c Lecturer, Cariology and Operative Dentistry Department, Graduate School of durable restorative and esthetically pleasing materials
Medical and Dental Sciences, Tokyo Medical and Dental University, Tokyo, which meet patient demands; in contrast, demands are de-
Japan. Idea, hypothesis, experimental design, proofread the manuscript.
creasing regarding other restorative materials.10 However,
d PhD Candidate, Cariology and Operative Dentistry Department, Graduate
School of Medical and Dental Sciences, Tokyo Medical and Dental University,
ceramic restorations are fragile, costly, and exert excessive
Tokyo, Japan. Performed statistical evaluation. wear on opposing enamel.3,7,23
e Professor, Cariology and Operative Dentistry Department, Graduate School of In the same context, indirect composite restorations are
Medical and Dental Sciences, Tokyo Medical and Dental University, Tokyo, becoming increasingly popular due to simplification of the
Japan. Supported the experiments, contributed substantially to the discus-
sion. fabrication process, reduced wear,5 reparability, and cost
effectiveness. Recently, dental manufacturers launched a
Correspondence: Tomohiro Takagaki, Cariology and Operative Dentistry Depart- CAD/CAM composite block (CCB) with different fabrication
ment, Graduate School of Medical and Dental Sciences, Tokyo Medical and
Dental University, 1-5-45, Yushima, Bunkyo-ku, Tokyo 113-8510, Japan. Tel: methods and in-house production. Most CCBs used to be
+81-3-5803-5483; e-mail: [email protected] exposed to extraordinary temperature alone or combined

Vol 20, No 4, 2018 317

Ali et al

with high pressure during polymerization to overcome flaws, crotensile bond strength (µTBS). In addition, the present
shrinkage, and operator-induced factors which occur at den- study monitored the impact of elapsed time after sandblast-
tal laboratories, as well as to increase homogeneity.5 Fur- ing on bond strength. The first null hypothesis tested was
thermore, regarding marginal adaptation, there was no dif- that the elapsed time after sandblasting had no effect on
ference after three years of clinical trials between porcelain the bonding performance, while the second null hypothesis
inlays and conventional composite-based CAD/CAM inlays, tested was that the different surface treatment agents had
but the latter possessed significantly better color stability.4 no influence on bond strength.
Recently, a nanofilled CCB has been developed based
on the filler press and monomer infiltration (FPMI) method.
The nanofillers are initially pressed into a green body before MATERIALS AND METHODS
being infiltrated by composite monomers in order to achieve
a uniform distribution of fillers.18 This CCB is composed of Materials
(62 wt%) densely packed silanated nanofillers, alumina filler The materials, components, manufacturers, batch num-
(20 nm), and silica filler (40 nm), and is embedded in resin bers, and application procedures used in this study are
monomers (24 wt%). listed in Table 1. The CCB used was Katana Avencia (Ka-
The bonding approaches must be examined, as CCBs tana Avencia block, Kuraray Noritake; Tokyo, Japan), and
have a greater degree of conversion than manually polymer- the composite cement was Panavia V5 (PV5, Kuraray Nori-
ized composite. In CCBs, unreacted monomers are few or take). 40% phosphoric acid (K-etchant gel, Kuraray Nori-
nonexistent.9,24 This minimizes the chemical adhesion abil- take) was used to clean the CCB surface. Ceramic Primer
ity of the composite cement to the CCB and necessitates (CP, Kuraray Noritake), Universal Bond (UB, Kuraray Nori-
adequate pretreatment of the CCB surface for bonding. take), and Clearfil Porcelain Bond Activator mixed with
According to manufacturers’ instructions, it is necessary to Clearfil tri-S Bond ND Quick (NDP, Kuraray Noritake) were
sandblast and silanize the CCB immediately before cementa- used as silane coupling agents for the CCB surfaces.
tion. Many studies have proposed that the combination of
sandblasting and silanization is a crucial step in achieving a Specimen Preparations
stable adhesion of lab-polymerized composite.16,21,27 The Figure 1 schematically illustrates specimen preparation.
sandblasting procedure is used to expose fresh surfaces and A CCB was cut into 72 slices by using a low-speed dia-
increase the micromechanical retention.22 Silanization is then mond-blade saw (Isomet, Buehler; Lake Bluff, IL, USA)
used to bind dissimilar molecules.30 under water irrigation with dimensions of approximately
Usually, the silane monomer is incorporated in a non- 14.5 × 14.5 × 2 mm. The slices were then wet ground with
aqueous solution and is hydrolysed by the other acidic ad- #600 SiC paper. After that, they were randomly distributed
hesive.8 Hydrolysation of the silane monomer is influenced into three groups – untreated and sandblasted with 50-µm
mainly by water and a lower pH. Therefore, silane mono- Al2O3 particles at 0.1 and 0.2 MPa (20 s, 10 mm distance)
mers incorporated in an aqueous medium have previously using a blasting machine (Basic Master, Renfert; Hilzingen,
been pre-hydrolysed and dehydrated, giving them a short Germany). All CCB slices were cleaned with 99% ethanol for
shelf-life.8,11,28 However, some manufacturers have re- 3 min in an ultrasonic bath. Then, according to the time
cently produced a primer containing silane monomer dis- elapsed after sandblasting, the slices were divided into two
solved in ethanol and/or mild acid without water.10 subgroups: same-day (S) and one-week (W) dry storage
Nonetheless, most studies have focused on the bonding under controlled laboratory conditions before cementation,
performance of CCBs without considering the effect of stor- where the temperature was set to 23.0 ± 0.5°C, with rela-
age time under laboratory conditions (“dry storage”) and tive humidity (RH) kept at 50% ± 5%.
the subsequent capability of γ-methacryloxypropyltrimethox
ysilane (γ-MPTS) to silanize after being incorporated with Bonding Procedures
adhesive into one bottle. So far, no study has considered Both CCB adherent surfaces were treated with 40% phos-
these factors and their consequences for bonding perfor- phoric acid for 20 s. After washing with water and air drying,
mance of CCBs. Nowadays, the surface treatment of CCBs the slices were then distributed randomly into three sub-
is manufacturer dependent. Some of them recommend groups according to the surface treatment: CP, UB, and
using universal bonding, while others recommend a sepa- NDP, in accordance with manufacturer’s instructions
rate silane coupling agent. Another important factor is that (Table 1). Afterwards, all CCB slices were cemented with
nearly all sandblasting procedures are conducted at labora- PV5 composite cement using a halogen light curing unit
tories, as not all practices and clinics have a chairside (Optilux 501, Demetron; Danbury, CT, USA) at 600 mW/
sandblaster, and the restorations are stored for up to 2 cm2 of light intensity for 60 s on each side. Specimens
weeks before placement. were then stored in distilled water at 37°C for 24 h.
Accordingly, this study was conducted to investigate the
bonding performance of CCBs and pretreatment factors, and µTBS Testing
evaluate the most efficient methods for pretreating CCBs by After the specimen had been stored for 24 h, they were cut
determining the appropriate sandblasting pressure used for perpendicularly into 1 × 1 mm sticks with a low-speed dia-
alumina-particle abrasion and silanization to enhance the mi- mond saw. The sticks (n = 10) were individually fixed to a

318 The Journal of Adhesive Dentistry

 Ali et al

Table 1 Composition of the materials used in the study and their applications procedure

Material Lot No. Composition Application procedures

Katana Avencia 000130 Mixed filler with colloidal silica (40 nm) and aluminum (20 nm) __
Block oxide, cured composites consisting of methacrylate monomer
(copolymer of urethane dimethacrylate and other methacrylate
monomers), pigments, filler content 62 wt%

Panavia V5 C80086 Paste A: bis-GMA, TEG-DMA, hydrophobic aromatic Apply to CCB surface using an auto-mix
dimethacrylate, hydrophilic aliphatic dimethacrylate, initiators, syringe, then light cure for 60 s or
accelerators, silanated barium glass filler, silanated chemical cure for 30 min in the dark.
fluoroalminosilicate glass filler, colloidal silica
Paste B: bis-GMA, hydrophobic aromatic dimethacrylate,
hydrophilic aliphatic dimethacrylate, silanated barium glass
filler, silanated alminium oxide filler, accelerators, dl-
camphorquinone, and pigments

K-etchant gel BP0054 40% phospholic acid gel, phosphoric acid, water, colloidal silica, Apply on the CCB surface for 20 s, rinse
pigment with water for 10 s and gently air dry

Clearfil Ceramic 1M0013 3-trimethoxysilylpropyl methacrylate, MDP, ethanol Apply on the CCB surface for 20 s and
Primer Plus gently air dry

Clearfil Universal 7M0010 HEMA, MDP, bis-GMA, ethanol, camphorquinone, hydrophilic Apply on the CCB surface for 10 s, mild
Bond aliphatic dimethacrylate, silane coupling agent, colloidal silica, air blowing for 5 s, light cure for 10 s
water, and accelerators

Clearfil Porcelain 5B0037 Bisphenol A polyethoxy dimethacrylate, 3-trimethoxysilylpropyl Dispense one drop each of porcelain
Bond Activator methacrylate bond activator and Clearfil tri-S Bond ND
Quick and mix them for 5 s. Apply it on
Clearfil tri-S B80055 Bis-GMA, MDP, HEMA, dimethacrylates, sodium fluoride, CCB surface for 5 s and light cure for
Bond ND Quick photoinitiator, water, micro filler 10 s

All materials manufactured by Kuraray Noritake, Tokyo, Japan. Abbreviations: bis-GMA: bisphenol A-glycidyl methacrylate; MDP: 10-methacryloyloxydecyl dihydro-
gen phosphate; HEMA: 2-hydroxyethyl methacrylate; TEG-DMA: triethyleneglycol dimethacrylate.

f Bonding with Panavia g Stored in distilled h Sectioned into

V5 composite cement water at 37°C for 24h 1-mm2 sticks
Light cured for 60 s
KATANA on each side
Avencia block

Stored for one week

in laboratory
a Isomet conditions
2 mm thick d
#600 SiC i Microtensile
test at 1 mm/min
Same-Day
crosshead speed
e 20 s 40% phosphoric
EZ-test (Shimadzu)
acid treatment, water
n = 10
rinsing, followed by UB
or CP or NDP application
b Sandblasting c Ultrasonically
(50 μm alumina) untreated, cleaned with
0.1 MPa or 0.2 MPa 99% ethanol
(3 min)
j Failure mode
analysis under
SEM

Fig 1 Sample preparation for microtensile bond strength test and SEM observation of failure mode.

testing apparatus with a cyanoacrylate glue (Model Repair II Failure Mode Analysis
Blue, Dentsply-Sankin; Tokyo, Japan) and then subjected to After specimen debonding, the failure mode was analyzed
µTBS testing using an EZ-Test machine (Shimadzu; Kyoto, using SEM. The sticks were mounted on specimen holders
Japan) at a crosshead speed of 1 mm/min. using carbon adhesion tape (Nisshin EM; Tokyo, Japan) and

Vol 20, No 4, 2018 319

Ali et al

KATANA
Avencia block

Untreated e f
a Surface • 20 s 40% phos-
Stored for one week
Isomet roughness phoric acid treat-
in laboratory conditions
2 mm thick 0.1 MPa measurement ment, water rins-
#600 SiC d (n=20) ing and air drying
(CLSM: VK-X150)
Same-Day • Contact angle
0.2 MPa measurement
(n=12)
b Sandblasting c Ultrasonically (VCA OPTIMA-XE)
(50 μm alumina) cleaned with
untreated, 0.1 MPa 99% ethanol
or 0.2 MPa (3 min)

Fig 2 Sample preparation for surface roughness test and contact angle measurement.

fixed with cyanoacrylate glue (Model Repair II Blue, air dried. Thereafter, a deionized water droplet was placed
Dentsply-Sankin). They were then gold sputter-coated and on the surface of each specimen and the contact angle (CA)
examined with scanning electron microscopy (SEM, JSM- was measured using a CA measuring device (VCA OPTIMA
5310LV, Jeol; Tokyo, Japan) at 200X magnification. The XE, Techscience; Koshigaya, Japan). The surface of the
failure modes were classified into four categories: (a) adhe- drop was constantly monitored and the CA was measured
sive failure between CCB and composite cement; (b) cohe- just after 20 s, when the droplet was stabilized. Each mea-
sive failure within composite cement; (c) cohesive failure surement was repeated at least 6 times (n = 12), and the
within CCB, and (d) mixed (type a + type b). mean value was reported.

Surface Roughness Analysis Statistical Analysis

Figure 2 illustrates specimen preparation for surface rough- The influence of three factors – sandblasting pressure, time
ness evaluation. Twelve CCB slices (2 mm width) were cut elapsed after sandblasting, and pretreatment methods –
using a low-speed diamond saw. The surfaces of the speci- was statistically analyzed with three-way ANOVA. The distri-
mens were wet ground using 600-grit SiC paper, the speci- bution of μTBS, CA measurement, and surface roughness
mens were then divided into three groups (untreated, data were first checked for normality utilizing the Kol-
0.1 MPa, 0.2 MPa), and cleaned with 99% ethanol for mogorov-Smirnov test, and then they were statistically ana-
3 min in an ultrasonic bath. They were then randomly di- lyzed with a two-way ANOVA using Bonferroni’s correction to
vided into two subgroups, a same-day group (untreated, test the influence of two factors of “sandblasting pressure”
0.1, 0.2 MPa) and 1-week group in which speciments were and “time elapsed after sandblasting” at a 95% confidence
kept under ordinary laboratory conditions for one week (un- level. All statistical procedures were carried out using SPSS
treated, 0.1, 0.2 MPa). Quantification of the surface rough- v 23.0 (IBM; Armonk, NY, USA).
ness parameter Sa (arithmetic mean deviation) was per-
formed using a laser scanning confocal microscope (CLSM,
VK-X150, Keysnce; Osaka, Japan) equipped with a 20X RESULTS
objective, and each surface was measured 10 times
(n = 20). μTBS
Table 2 shows the mean µTBS and standard deviations. All
Contact Angle Measurement groups registered a significant drop in μTBS after one week
Figure 2 also shows specimen preparation for contact angle (p < 0.01), except for the UB group, which had a more sta-
measurement. Twelve CCB slices (2 mm width) were cut ble μTBS with no significant difference detected at 0.2 MPa
with a low-speed diamond saw. The surfaces of the speci- after one week. Regardless of the pretreatment methods,
mens were wet ground using 600-grit SiC paper. They were the overall results showed a significant difference between
then divided into three groups (untreated, 0.1 MPa, and untreated and sandblasted groups. With the exclusion of
0.2 MPa), and cleaned with 99% ethanol for 3 min in an the UB group, which showed no significant difference be-
ultrasonic bath. Subsequently, they were randomly divided tween untreated, 0.1 MPa, and 0.2 MPa of the S group and
into two subgroups, a same-day group (untreated, 0.1, between 0.1 MPa and 0.2 MPa of the W group. In the W
0.2 MPa) and 1-week group in which specimens were kept group, no significant difference occurred between 0.1 MPa
under ordinary laboratory conditions for one week (un- and 0.2 MPa for CP and UB groups, while the NDP groups
treated, 0.1, 0.2 MPa). After that, they were treated with showed a significant difference. NDP groups (S and W)
40% phosphoric acid for 20 s, rinsed with water spray, and showed a higher μTBS compared to CP and UB.

320 The Journal of Adhesive Dentistry

 Ali et al

Table 2 Microtensile bond strength means ± SD (MPa) by time elapsed, surface treatment, and pre-cementation
sandblasting pressure

Time elapsed Surface treatment Untreated 0.1 MPa sandblasting pressure 0.2 MPa sandblasting pressure
S CP 38.4 ± 6.5a,B 52.6 ± 6.5c,B 44.6 ± 5.6e,B
UB 38.9 ± 5.1a,B 43.8 ± 10.0a,B 42.5 ± 7.5a,B
NDP 45.8 ± 3.9a,B 52.0 ± 4.8b,B 59.0 ± 4.9c,B

W CP 26.7 ± 4.0b,A 35.2 ± 3.2c,A 31.6 ± 2.7c,A

UB 27.8 ± 1.6b,A 39.6 ± 7.5c,B 35.3 ± 9.5c,A
NDP 30.3 ± 3.9b,A 44.4 ± 3.8a,A 50.6 ± 3.3c,A

n = 10. Same superscript letters indicate no statistically significant differences (p > 0.05). Lowercase letters show the sandblasting effect (untreated,
0.1 MPa, 0.2 MPa) and capital letters show the time-elapsed effect (S, W) for each material.

Table 3 Failure mode distribution

Time elapsed Surface treatment Untreated 0.1 MPa sandblasting pressure 0.2 MPa sandblasting pressure
S CP [6/0/0/4] [1/3/4/2] [5/1/4/0]
UB [9/0/0/1] [2/1/6/1] [3/0/1/6]
NDP [8/0/0/2] [2/4/0/4] [1/2/0/7]

W CP [3/6/0/1] [6/3/0/1] [6/4/0/0]

UB [9/0/0/1] [6/4/0/0] [5/4/0/1]
NDP [10/0/0/0] [8/1/0/1] [7/1/0/2]

Numbers of specimens per fracture mode [A/B/C/D] in square brackets: [A] adhesive failure between CCB and composite cement; [B] cohesive failure within
composite cement; [C] cohesive failure within CCB; [D] mixed (type A + type B).

a b

Fig 3 Micrographs of the failure types, 200X

magnification. (a): adhesive failure between
CCB and composite cement; (b): cohesive fail-
ure within composite cement; (c): cohesive
failure within CCB; (d): mixed: cohesive failure
within composite cement plus adhesive failure
c d
between CCB and composite cement.

Failure Mode Analysis failure within the composite cement (type b) in addition to
The results of the failure mode analysis are summarized in cohesive failure within the CCB (type c) and/or mixed failure
Table 3 and Fig 3. In the untreated group (CP, UB, and NDP) (type d) increased. However, the UB and NDP groups at
for both S and W time periods, the failure mode analysis 0.2 MPa tended to show predominantly mixed failures (type
showed a majority of adhesive failure between the CCB and d). Regardless of the sandblasting, all W groups showed
composite cement (type a). In the S group of CP, UB and predominantly adhesive failure between the CCB and the
NDP, as the sandblasting pressure increased, the cohesive composite cement (type a).

Vol 20, No 4, 2018 321

Ali et al

Table 4 Means and standard deviations of surface Table 5 Means and standard deviations of contact an-
roughness (µm) gles in degrees

Time Untreated 0.1 MPa 0.2 MPa Time Untreated 0.1 MPa 0.2 MPa
elapsed elapsed
S 1.2 ± 0.1a,A 2.0 ± 0.2b,B 2.4 ± 0.4c,C S 61.1 ± 2.6a,A 78.8 ± 2.4b,B 81.8 ± 5.7b,B

W 1.2 ± 0.2a,A 2.1 ± 0.1b,B 2.4 ± 0.5c,C W 58.4 ± 4.3c,A 74.4 ± 3.2d,D 71.8 ± 3.3d,E

n = 20. Same superscript letters indicate no statistically significant differ- n = 12. Same superscript letters indicate no statistically significant differ-
ence (p > 0.05). Lowercase letters show the significance in rows, and ence (p > 0.05). Lowercase letters show the significance in rows, and
capital letters show the significance in columns for each group. capital letters show the significance in columns for each group.

Surface Roughness Analysis air at the laboratory site is a major concern. In this study,
The surface roughness results after sandblasting are sum- the temperature and relative humidity were set to
marized in Table 4. Surface roughness differed statistically 23.0 ± 0.5°C and 50 ± 5%, respectively. However, storing
significantly after sandblasting with alumina between all the samples in a dry environment does not mean stable
groups (p < 0.01), while no significant differences were ob- conditions, as water may be absorbed from the surrounding
served after 1 week (p > 0.05). environment. The amount of absorbed water into CCB sur-
faces is dependent on RH, room temperature, storage pe-
Contact Angle Measurement riod, and the hydrophilicity of resin monomers.1,14,15
Table 5 shows the CA (θ) of each group and the standard The conventional parameter for evaluating the wettability
deviations. All W (sandblasted) groups exhibited signifi- of material is to measure the CA of a drop of water.29 The
cantly lower CA than did the S group (p < 0.05). The CA in- surface texture, surface energy of the solid substrate, sur-
creased with sandblasting. On the other hand, there was no face tension of the liquid, and the reaction of liquid-solid
statistically significant difference between S and W groups interface impacts CA measurements.13
at blasting pressures of 0.1 MPa and 0.2 MPa. Many factors influence the wettability and surface rough-
ness, for example, the characteristics of the composite
filler particles and filler loading.20,25 In this study, the CA of
DISCUSSION the untreated group was 60 degrees, but with intensifying
the blasting pressure, the CA also increased and therefore
Previous research generally confirms air abrasion using the wettability decreased. However, when the samples were
50-µm alumina particles (Al2O3) as the most effective dry-stored for 1 week under laboratory conditions, the CCB
method to roughen indirect composite restorations.2,22 wettability increased significantly across all sandblasted
CLSM observation of the CCB surfaces revealed that the groups. The results of this study showed that the surface
surface roughness increased significantly with increasing roughness increased with sandblasting; therefore, the sur-
sandblasting pressure. However, there were no significant face irregularities increased and the µTBS improved, but
differences between the S and W groups. This study used after 1 week, the µTBS and the CA decreased significantly.
air abrasion with alumina particles at 0.1 MPa and a maxi- This could be attributed to the time elapsed after sand-
mum of 0.2 MPa pressure, as specified by Yoshihara et blasting prior to adhesion, which may affect bond strength
al,27 due to the initiation of small cracks inside the CCB due to the miniscule water droplets that may have been
surface after sandblasting at 0.2 MPa. trapped in the grooves and the micropores formed by the
Silanization is an effective means of achieving chemical blasting process. Those tiny drops of surrounding humidity
adhesion between composite cement and CCB.26 However, promote the wettability of CCBs through hydrogen bonds
silane monomer in aqueous solution, as is the case with formed by intermolecular forces to form new macrodrops. In
universal bonding, has proven to be unstable; it already hy- addition, the presence of a thin layer of moisture impairs
drolyzes inside the bottle. As the silane monomer reacts the bond strength and prevents monomers from penetrating
with water, it then hydrolyzes to silanol and later bonds the underlying layer.
chemically with glass; however, it might convert to an oligo- Regardless of the surface treatment applied after sand-
mer and lose the ability to bond to glass.8,11,12,28 In the blasting, the time elapsed after sandblasting was shown to
present study, the µTBS demonstrated that the highest influence bond strength. The first null hypothesis of this
bond strength was obtained after sandblasting at 0.1 or study was thus rejected.
0.2 MPa in the S group. It was noted that NDP showed the In agreement with Yoshihara et al,28 in this study, the
highest bond strength among all pretreatments tested here. separate silane primer (CP) or freshly mixed silane plus ad-
Sandblasting with alumina particles followed immediately hesive (NDP) yielded much higher µTBS than did UB in the
by silanization is an appropriate treatment and is recom- S group. The µTBS of CP or NDP improved significantly with
mended by the manufacturer; however, storing the CCB sandblasting due to the deeper penetration of composite
after sandblasting or exposing the CCB surface to ambient cement into microretentive areas through effective silane

322 The Journal of Adhesive Dentistry

 Ali et al

coupling.6,8,11,22 In contrast, the UB group (S) showed no the mean µTBS, with the exclusion of non-separated silane
statistically significant differences after increasing sand- coupling agents, as was displayed by the stable perfor-
blasting pressure, mainly because the silane monomer was mance of µTBS after similar storage.
previously dehydrated. Despite the considerable improve-
ment of bond strength with NDP or CP in the S group, both
of them showed a significant bond-strength reduction after ACKNOWLEDGMENTS
1 week. However, the significant reduction was higher in This study was supported by JSPS KAKENHI (Grant No. 17K11701).
the CP than in the NDP group. In the case of NDP, the si-
lane coupling agent in the first bottle (porcelain bond activa-
tor) was freshly activated (hydrolysis) by water in the sec- REFERENCES
ond bottle (Clearfil tri-S Bond ND Quick), while activation of
1. Asay DB, Kim SH. Evolution of the adsorbed water layer structure on sili-
CP silane monomers depended on the existence of water con oxide at room temperature. J Phys Chem B 2005;109:16760-16763.
on the CCB surface as well as the lack of polymerization 2. da Costa TR, Serrano AM, Atman AP, Loguercio AD, Reis A. Durability of
catalyst to influence chemical adhesion.17 Noda et al17 con- composite repair using different surface treatments. J  Dent
2012;40:513-521.
firmed that CP showed a dramatic reduction in bond
3. Fasbinder DJ. Materials for chairside CAD/CAM restorations. Compend
strength after thermocycling in comparison to freshly mixed Contin Educ Dent 2010;31:702-4, 706, 708-9.
silane monomer. 4. Fasbinder DJ, Dennison JB, Heys DR, Lampe K. The clinical performance
SEM observations of the failure patterns provided addi- of CAD/CAM-generated composite inlays. J  Am Dent Assoc
2005;136:1714-1723.
tional evidence. Without mechanical interlocking, the frac- 5. Giordano R. Materials for chairside CAD/CAM-produced restorations.
ture patterns of untreated groups (S and W) revealed that J Am Dent Assoc 2006;137 Suppl:14S-21S.
failure mainly occurred between CCB and the composite 6. Hemadri M, Saritha G, Rajasekhar V, Pachlag KA, Purushotham R, Reddy
VK. Shear bond strength of repaired composites using surface treat-
cement (type a). Irrespective of sandblasting, all groups ments and repair materials: an in vitro study. J  Int Oral Health
showed predominantly adhesive failure between CCB and 2014;6:22-25.
composite cement (type a) after one week, as the moisture 7. Lee A, Swain M, He L, Lyons K. Wear behavior of human enamel against
lithium disilicate glass ceramic and type III gold. J  Prosthet Dent
affects the adhesion process. After sandblasting, the S 2014;112:1399-1405.
group (CP, UB, and NDP) showed more cohesive failure 8. Lung CY, Matinlinna JP. Aspects of silane coupling agents and surface
within the CCB (type c) or mixed failure (type d), and this conditioning in dentistry: an overview. Dent Mater 2012;28:467-477.
confirms that mechanical interlocking and/or chemical 9. Mainjot AK, Dupont NM, Oudkerk JC, Dewael TY, Sadoun MJ. From arti-
sanal to CAD-CAM blocks: state of the art of indirect composites. J Dent
bonding were achieved thanks to silane easily reaching the Res 2016;95:487-495.
inorganic part of CCB. Looking at the W group, the de- 10. Makhija SK, Lawson NC, Gilbert GH, Litaker MS, McClelland JA, Louis
creased µTBS and CA and an increase of adhesive failure DR, Gordan VV,  Pihlstrom DJ,  Meyerowitz C,  Mungia R,  McCracken MS.
Dentist material selection for single-unit crowns: findings from the Na-
between CCB and the composite cement may possibly be tional Dental Practice-Based Research Network. J Dent 2016;55:40-47.
explained by hydrogen bonding between water and silica, 11. Matinlinna JP, Lung CYK, Tsoi JKH. Silane adhesion mechanism in dental ap-
plications and surface treatments: A review. Dent Mater 2018;34:13-28.
which creates an invisible layer of moisture that may have
12. Matinlinna JP, Vallittu PK. Bonding of resin composites to etchable ce-
obstructed covalent bond formation at the silane-silica inter- ramic surfaces – an insight review of the chemical aspects on surface
face.19 This influences the adherend surfaces of the CCB conditioning. J Oral Rehabil 2007;34:622-630.
and reduces the penetration of the silane and luting cement 13. Milleding P, Gerdes S, Holmberg K, Karlsson S. Surface energy of noncor-
roded and corroded dental ceramic materials before and after contact
into the microretentive areas. However, the UB group was with salivary proteins. Eur J Oral Sci 2003;107:384-392.
unaffected by this layer, as it does not depend on silaniza- 14. Musanje L, Darvell BW. Aspects of water sorption from the air, water and
tion. artificial saliva in resin composite restorative materials. Dent Mater
2003;19:414-422.
The second objective of this study was to evaluate the 15. Musanje L, Shu M, Darvell BW. Water sorption and mechanical behaviour
silane coupling agent performance utilizing different applica- of cosmetic direct restorative materials in artificial saliva. Dent Mater
tion methods. Regardless of the time elapsed after sand- 2001;17:394-401.
16. Nobuaki A, Keiichi Y, Takashi S. Effects of air abrasion with alumina or
blasting, freshly mixed silane monomer (NDP) showed ade- glass beads on surface characteristics of CAD/CAM composite materials
quate bonding performance between the CCB and and the bond strength of resin cements. J Appl Oral Sci 2015;23:629-636.
composite cement among others; hence, the second null 17. Noda Y, Nakajima M, Takahashi M, Mamanee T, Hosaka K, Takagaki T,
Ikeda M, Foxton RM, Tagami J. The effect of five kinds of surface treat-
hypothesis was rejected. ment agents on the bond strength to various ceramics with thermocycle
One limitation of the present study was that only a single aging. Dent Mater J 2017;36:755-761.
type of CCB was evaluated. Further studies should clarify 18. Okada K, Kameya T, Ishino H, Hayakawa T. A novel technique for prepar-
ing dental CAD/CAM composite resin blocks using the filler press and
whether a shorter duration of dry storage after sandblasting monomer infiltration method. Dent Mater J 2014;33:203-209.
is also as effective as one-week dry storage. 19. Roulet JF, Söderholm KJ, Longmate J. Effects of treatment and storage
conditions on ceramic/composite bond strength. J  Dent Res
1995;74:381-387.
20. Shintani H, Satou N, Yukihiro A, Satou J, Yamane I, Kouzai T, Andou
CONCLUSION T, Kai M, Hayashihara H, Inoue T. Water sorption, solubility and staining
properties of microfilled resins polished by various methods. Dent Mater
J 1985;4:54-62.
The sandblasting with alumina at 0.1 MPa or 0.2 MPa with
21. Soares CJ, Giannini M, Oliveira MT, Paulillo LA, Martins LR. Effect of sur-
separated silane improved the µTBS; however, one-week face treatments of laboratory-fabricated composites on the microtensile
dry storage had a statistically significant negative effect on bond strength to a luting resin cement. J Appl Oral Sci 2004;12:45-50.

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22. Spitznagel FA, Horvath SD, Guess PC, Blatz MB. Resin bond to indirect 28. Yoshihara K, Nagaoka N, Sonoda A, Maruo Y, Makita Y, Okihara T, Irie M,
composite and new ceramic/polymer materials: a review of the literature. Yoshida Y, Van Meerbeek B. Effectiveness and stability of silane coupling
J Esthet Restor Dent 2014;26:382-393. agent incorporated in ‘universal’ adhesives. Dent Mater 2016;32:
23. Sripetchdanond J, Leevailoj C. Wear of human enamel opposing mono- 1218-1225.
lithic zirconia, glass ceramic, and composite resin: an in vitro study. 29. Yuan Y LT. Contact angle and wetting properties. In: Bracco G, Holst B
J Prosthet Dent 2014;112:1141-1150. (eds). Surface Science Techniques. Berlin: Springer, 2013:3-34.
24. Stawarczyk B, Basler T, Ender A, Roos M, Özcan M, Hämmerle C. Effect 30. Zaghloul H, Elkassas DW, Haridy MF. Effect of incorporation of silane in
of surface conditioning with airborne-particle abrasion on the tensile the bonding agent on the repair potential of machinable esthetic blocks.
strength of polymeric CAD/CAM crowns luted with self-adhesive and con- Eur J Dent 2014;8:44-52.
ventional resin cements. J Prosthet Dent 2012;107:94-101.
25. Yap AU, Wee KE. Effects of cyclic temperature changes on water sorption
and solubility of composite restoratives. Oper Dent 2002;27:147-153.
26. Yoshida K, Kamada K, Atsuta M. Effects of two silane coupling agents, a Clinical relevance: Clinically, blasting the inner sur-
bonding agent, and thermal cycling on the bond strength of a CAD/CAM faces of the CCB crown at 0.1 or 0.2 MPa pressure and
composite material cemented with two resin luting agents. J  Prosthet
Dent 2001;85:184-189. silanization immediately prior to cementation using sep-
27. Yoshihara K, Nagaoka N, Maruo Y, Nishigawa G, Irie M, Yoshida Y, Van arated silane coupling agents is recommended to ob-
Meerbeek B. Sandblasting may damage the surface of composite CAD- tain stable chemical adhesion.
CAM blocks. Dent Mater 2017;33:e124-e135.

324 The Journal of Adhesive Dentistry