Bond Strength of Novel CAD/CAM Restorative

Materials to Self-Adhesive Resin Cement:

The Effect of Surface Treatments
Shaymaa E. Elsaka

Purpose: To evaluate the effect of different surface treatments on the microtensile bond strength (μTBS) of
novel CAD/CAM restorative materials to self-adhesive resin cement.
Materials and Methods: Two types of CAD/CAM restorative materials (Vita Enamic [VE] and Lava Ultimate
[LU]) were used. The specimens were divided into five groups in each test according to the surface treatment
performed; Gr 1 (control; no treatment), Gr 2 (sandblasted [SB]), Gr 3 (SB + silane [S]), Gr 4 (hydrofluoric acid
[HF]), and Gr 5 (HF + S). A dual-curing self-adhesive resin cement (Bifix SE [BF]) was applied to each group for
testing the adhesion after 24 h of storage in distilled water or after 30 days using the μTBS test. Following frac-
ture testing, specimens were examined with a stereomicroscope and SEM. Surface roughness and morphology
of the CAD/CAM restorative materials were characterized after treatment. Data were analyzed using ANOVA and
Tukey’s test.
Results: The surface treatment, type of CAD/CAM restorative material, and water storage periods showed a sig-
nificant effect on the μTBS (p < 0.001). For the LU/BF system, there was no significant difference in the bond
strength values between different surface treatments (p > 0.05). On the other hand, for the VE/BF system, sur-
face treatment with HF + S showed higher bond strength values compared with SB and HF surface treatments
(p < 0.05). Surface roughness and SEM analyses showed that the surface topography of CAD/CAM restorative
materials was modified after treatments.
Conclusion: The effect of surface treatments on the bond strength of novel CAD/CAM restorative materials to
resin cement is material dependent. The VE/BF CAD/CAM material provided higher bond strength values com-
pared with the LU/BF CAD/CAM material.
Keywords: adhesion, microtensile, polymer-infiltrated ceramic network, resin cement, resin nanoceramic, sur-
face roughness, surface treatments.

J Adhes Dent 2014; 16: 531–540. Submitted for publication: 30.01.14; accepted for publication: 21.08.14
doi: 10.3290/j.jad.a33198

T he use of dental CAD/CAM restorative materials for

indirect restorations has recently increased consider-
ably. Ceramics and composite resins are the two main
groups of CAD/CAM restorative materials.10 Ceramic
restorations have several advantages, including highly
esthetic appearance, wear resistance, biocompatibility,
and color stability.26,40 However, ceramics are brittle,
causing excessive wear to opposing dentition, and sus-
ceptible to fracture due to the formation of flaws or de-
fects in the intaglio surfaces.3,10,26 On the other hand,
indirect composite restorations are more compliant and
Assistant Professor, Department of Dental Biomaterials, Faculty of Dentistry,
Mansoura University, Mansoura, Egypt.
Correspondence: Shaymaa E. Elsaka, Department of Dental Biomaterials,
Faculty of Dentistry, Mansoura University, Mansoura PC 35516, Egypt. Tel:
+20-100-410-1558. e-mail: shaymanaghy@mans.edu.eg
soft, easier to finish and polish, create less wear on op-
posing dentition, and are conducive to making add-on
adjustments, although they experience high wear.10,24
Consequently, the development of restorative materials
that combine the advantages of ceramics and compos-
ites will enhance the properties and longevity of indirect
esthetic restorations.10
Recently, a novel CAD/CAM restorative material for
indirect restorations has been developed, based on a
polymer-infiltrated ceramic network material (PICN).10
The PICN restorative material consists of a dominant
ceramic network (86 wt%) which is reinforced by an
acrylate polymer network (14 wt%) with both networks
fully penetrating one another.46 It was manufactured
by introducing a polymeric second phase with a lower
modulus of elasticiy into ceramic networks.9 Accord-
ingly, the PICN restorative material combines the posi-
tive characteristics of ceramics and resin-based com-

Vol 16, No 6, 2014 531

Elsaka
Table 1 Materials used in this study
Material Product and composition*
CAD/CAM Vita Enamic (86 wt% feldspar ceramic, 14 wt% polymer)
restorative
material Lava Ultimate (80 wt% nanoceramic, 20 wt% resin)
Dual-curing Bifix SE – Base: bis-GMA, UDMA, acidic phosphate monomers,
resin cement glycerindimethacrylate, benzoyl peroxide, aerosol silica, hydroxypro-
pylmethacrylate, catalysts, initiators, stabilizers, glass fillers (70
wt%); catalyst: UDMA, glycerindimethacrylate, catalysts, initiators
Composite Filtek Z250 Universal Restorative, A2 Shade – organic matrix: TEG-
resin DMA < 1–5%, bis-GMA < 1–5%, bis-EMA 5–10%, UDMA 5–10%;
fillers: 0.01−3.5 μm silica/zirconia particles 82 wt%
*Manufacturers’ data. Bis-GMA: bisphenol-A-glycidylmethacrylate; UDMA: urethane dimethacrylate; TEG-DMA: triethyleneglycol dimethacrylate; bis-EMA:
bisphenol-A polyethyleneglycol dietherdimethacrylate.
posites.46 It has been reported that the PICN CAD/CAM
is characterized by reduced brittleness, rigidity, and
hardness, together with enhanced flexibility, fracture
toughness, and improved machinability compared with
ceramics.10 In addition, it was found that the mechani-
cal properties of the PICN were close to those of human
enamel and dentin.10,22,23
Another CAD/CAM-system-machinable dental mater-
ial has been developed to meet the esthetic demands
of prosthetic restorations. Termed resin nanoceramic
(RNC) and based on nanotechnology, it is composed of
80 wt% zirconia/silica nanoceramic particles embedded
in a highly cross-linked resin matrix (20 wt%).28 The RNC
restorative materials contains silica nanomers (20 nm),
zirconia nanomers (4 to 11 nm), nanocluster particles de-
rived from the nanomers (0.6 to 10 μm), silane coupling
agent, and resin matrix.29 In terms of materials science,
the RNC CAD/CAM restorative material belongs in the
resin composite category.8
Bonding of indirect esthetic restorations to the tooth
structure remains a challenging matter, as the bonding
interfaces are increased with the indirect restorative pro-
cedure. The bonding interfaces include the tooth structure
and the fitting surface of the restoration. Consequently, to
establish a strong, durable bond, appropriate treatment
of the respective surfaces is crucial.14 Non-destructive,
simple, and applicable methods for pre-treating indirect
restoration surfaces would be clinically beneficial.35 In
addition, using adhesive cements enhances the fracture
resistance of indirect esthetic restorations.14 It is es-
sential to improve the bond strength between indirect
restorative materials and cements, since they are the
principal factors in the success of resin-bonded fixed den-
tal prostheses.16,33 To date, no study has determined the
effect of surface treatments to enhance the adhesion of
the recently introduced CAD/CAM PICN and RNC restora-
tive materials to resin cement. Accordingly, the present
study aimed to evaluate the effect of different surface
treatments on the microtensile bond strength of CAD/
CAM PICN and RNC restorative materials to self-adhesive
resin cement.
532
Lot Manufacturer
37990 Vita Zahnfabrik; Bad Säckingen, Germany
N392136 3M ESPE; St Paul, MN, USA
1322421 VOCO; Cuxhaven, Germany
8LXJ 3M ESPE
MATERIALS AND METHODS
Two types of CAD/CAM restorative materials were used
in this study: Vita Enamic (VE) and Lava Ultimate (LU).
The manufacturers and the compositions of the mater-
ials are presented in Table 1.
Grouping of specimens
VE and LU specimens were cut from their respective
blocks using a water-cooled diamond blade (Diamond
Wafering Blade, Buehler; Lake Bluff, IL, USA) with a
low-speed cutting saw (Isomet, Buehler) to produce
specimens with the required dimensions for each test.
The specimens from each CAD/CAM restorative ma-
terial block were wet ground on only one surface using
600-grit silicon carbide (SiC) paper (Leco; St Joseph, MI,
USA) and then ultrasonically cleaned (Sonorex, Bande-
lin; Berlin, Germany) in distilled water for 5  min. Then,
the specimens in each test were divided into 5 groups
according to the surface treatment performed.
y Group 1: Control (C; no treatment). The specimens
were exposed only to grinding and ultrasonic cleaning
as mentioned above.
y Group 2: Sandblasted (SB). The specimens were
abraded with 110-μm aluminum-oxide (Al 2O3) par-
ticles with a dental airborne-particle abrasion unit (Mi-
cro-Blaster, Daedong Industrial; Daegu, Korea) was
applied for 20 s at a pressure of 2 bar with a dis-
tance of 15 mm between the nozzle and the surface.
Then, the specimens were ultrasonically cleaned for
5 min in distilled water and air dried.
y Group 3: Sandblasted + silane (SB + S). The speci-
mens were sandblasted as in group 2, and then a
silane coupling agent (Ultradent silane, Ultradent
Products; South Jordan, UT, USA) was applied on the
surface of the specimen with a brush and air dried for
1 min.
y Group 4: Hydrofluoric acid (HF). The specimens were
etched with hydrofluoric acid (Ultradent Porcelain Etch
9% Buffered, Ultradent) for 1 min, then rinsed for
1 min and air dried.
The Journal of Adhesive Dentistry

y Group 5: Hydrofluoric acid + silane (HF + S). The
specimens were etched with hydrofluoric acid as in
group 4, and then a silane coupling agent was ap-
plied on the surface of the specimen with a brush
and air dried for 1 min.
Microtensile Bond Strength (μTBS) Test
A total of fifteen blocks from each CAD/CAM restora-
tive material (10 mm × 10 mm × 10 mm) were pre-
pared and divided into 5 test groups according to
the surface treatments applied (n = 3/group). Each
block was duplicated in composite resin (Filtek Z250;
Table 1) with the same dimensions using a mold made
of a silicone impression material (Express, 3M ESPE;
St Paul, MN, USA). Composite resin layers were incre-
mentally (2 mm) condensed into the mold until it was
full, and each layer was cured for 40 s with an LED
light-curing unit (Elipar S10, 3M ESPE; light output:
1200 mW/cm2). A glass microscope slide was used to
compress the last increment to obtain a flat surface.
After that, the specimen was removed from the mold
and an additional 40 s of irradiation was performed on
the areas that were previously in contact with the sili-
cone mold. The bonding surfaces of these blocks were
wet ground using 600-grit SiC paper. One composite
resin block was constructed for each CAD/CAM re-
storative material block.11,21
Luting procedure
The composite resin blocks were bonded to the treated
CAD/CAM restorative material block surfaces using a
dual-curing self-adhesive resin cement (Bifix SE; BF)
(Table 1) according to the manufacturer’s instructions.
A standardized constant pressure of 1 kg (0.098  MPa)
was applied to lute CAD/CAM restorative material/com-
posite blocks using a customized metallic tool. The com-
pressive force was applied for the first 5  min, leaving
the material to set in the self-curing modality. After that,
the specimen was light cured for 40 s from each side to
ensure optimal polymerization. The bonded specimens
were stored in distilled water for 24 h at 37°C prior to
μTBS testing.11,21
After that, the specimens were vertically sectioned into
serial slabs and further into beams with cross-sectional
areas of approximately 1 mm2 using a water-cooled dia-
mond blade with a low-speed cutting saw. Twenty beams
were obtained from each block. The peripheral slices were
excluded, as the results could be influenced by either
an excess or a deficient amount of resin cement at the
interface.36 Ten of them were tested after 24 h storage
in distilled water at 37°C, and the other ten beams were
tested after 30 days storage in distilled water at 37°C.
The specimens were attached to a Bencor Multi-T testing
device (Danville Engineering; San Ramon, CA, USA) using
a cyanocrylate adhesive (Zapit, Dental Ventures of Amer-
ica; Anaheim, CA, USA) and stressed to failure in tension
using a universal testing machine (Model TT-B, Instron;
Canton, MA, USA) at a crosshead speed of 0.5 mm/min.
The load at failure (N) and the surface area (mm2) for each
specimen was used to calculate the μTBS in MPa. A digital
Vol 16, No 6, 2014
Elsaka
caliper (Mitutoyo; Kawasaki, Japan) was used to measure
the cross-sectional area at the site of fracture. Statistical
analysis (SPSS 15.0; Chicago, IL, USA) of the μTBS (MPa)
values was performed using a three-way ANOVA consider-
ing three factors (surface treatment, type of CAD/CAM
restorative material, and water storage periods) and their
interaction. Multiple comparisons were made by Tukey’s
test. Statistical significance was set at the 0.05 prob-
ability level.
Debonded specimens were examined under a ster-
eomicroscope (Olympus SZX-ILLB100-Olympus Optical;
Tokyo, Japan) at 50X magnification to determine the
fracture pattern. Representative fractured specimens
from each group were rinsed with 96% ethanol and air
dried, mounted on metallic stubs, sputtered with a gold
layer (SPI-Module Sputter Coater, Structure Probe; West
Chester, PA, USA), and then examined under a scan-
ning electron microscopy (SEM) (JSM-6510LV, JEOL; To-
kyo, Japan) at 500X magnification. The modes of failure
were classified according to one of four types: type 1,
adhesive failure (complete CAD/CAM restorative mater-
ial surface was visible); type  2, mixed failure in CAD/
CAM restorative material surface and luting resin (par-
tial CAD/CAM restorative material surface and a partial
luting resin cover were visible); type 3, cohesive failure
within the luting resin layer (almost all of the fracture
surface was covered with luting resin); type  4, mixed
failure in CAD/CAM restorative material surface, luting
resin, and resin composite (both luting resin and resin
composite were detected on the CAD/CAM restorative
material surface).7
Surface Roughness Measurement
The surface roughness of the treated VE and LU
plates (10 mm × 10 mm × 2 mm) (n = 10/group) was
measured using a portable surface 2D texture-measur-
ing instrument (Surftest SJ-201 P, Mitutoyo) to mea-
sure R a (average roughness height) in micrometers
(μm). A diamond stylus with a tip radius of 5 μm was
used for the measurements. The detector moves over
the specimen with a driving speed of 0.25 mm/s for
a measured length of 1.25 mm. Ra for each specimen
was measured at five different sites and the mean
roughness average was then calculated. Mean surface
roughness values were analyzed using two-way ANOVA
considering two factors (surface treatment and type
of CAD/CAM restorative material) and their interac-
tion. Multiple comparisons were made by Tukey’s test.
Statistical significance was set at the 0.05 probability
level.
SEM Evaluation
Three representative specimens from each group of
the VE and LU plates (10 mm × 10 mm × 2 mm) were
rinsed with 96% ethanol and air dried, mounted on me-
tallic stubs, sputtered with a gold layer, and then exam-
ined under a SEM at magnification of 1000X to observe
the features of the treated surfaces.
533
Elsaka
Table 2 Mean (standard deviation) of the μTBS (MPa) of CAD/CAM restorative material/luting resin combinations
with different treatments
Surface treatment
24 h
C 18.67 (3.1)aA
SB 21.87 (3.75)bA
SB + S 24.95 (3.79)cdA
HF 23.86 (3.19)bdA
HF + S 27.47 (4.28)cA
Mean values represented with same superscript uppercase letters (row) or lowercase letters (column) are not significantly different according to Tukey’s test
(p > 0.05).
RESULTS
Three-way ANOVA of the μTBS testing data (surface
treatment, type of CAD/CAM restorative material, and
water storage periods) revealed that the bond strength
was significantly affected by the surface treatment,
type of CAD/CAM restorative material, and water stor-
age periods (p < 0.001). There were significant inter-
actions between surface treatment and type of CAD/
CAM restorative material (p < 0.001). However, there
were no significant interactions between type of CAD/
CAM restorative material and water storage periods
(p = 0.06), the surface treatment and water storage
periods (p = 0.854), or the type of CAD/CAM restorative
material, water storage periods, and surface treatment
(p = 0.644).
The mean μTBS values (MPa) and standard devia-
tions are presented in Table 2. The bond strength values
achieved with HF + S, SB + S, HF, and SB groups were
significantly higher compared with the control groups for
both types of CAD/CAM restorative materials under differ-
ent aging periods (p < 0.05). Regarding the type of CAD/
CAM restorative material, there was a significant differ-
ence in the bond strength values between VE and LU after
different aging periods (p < 0.05). For the LU/BF system,
there was no significant difference in the bond strength
values between different surface treatments under differ-
ent aging periods (p > 0.05). On the other hand, for the
VE/BF system, surface treatment with HF + S showed
higher bond strength values compared with SB and HF sur-
face treatments under different aging periods (p < 0.05).
Additionally, for the VE/BF system, no significant differ-
ence in bond strengths was found between either HF + S
and SB + S (p = 0.239) or HF and SB surface treatments
(p = 0.699). After 30 days of water storage, the μTBS
of BF to VE and LU significantly decreased in all groups
(p < 0.05) (Table 2).
Regarding the failure modes, mixed failures of type 2
(both a part of the CAD/CAM restorative material surface
and partial luting resin coverage were visible, 46.34%)
were observed in all tested groups. In addition, cohesive
534
VE/BF LU/BF
30 days 24 h 30 days
12.67 (2.13)aB 11.99 (2.52)aB 8.28 (1.99)aC
16.71 (3.42)bB 16.93 (3.66)bB 13.49 (3.4)bC
19.48 (3.18)bcB 18.82 (3.69)bB 13.88 (3.47)bC
18.86 (3.31)bB 18.35 (2.84)bB 13.45 (3.24)bC
22.21 (3.04)cB 19.21 (3.87)bC 14.35 (2.56)bD
failure in the luting resin (type 3, 21.99%), mixed failures
of type 4 (both luting resin and resin composite were
detected on the CAD/CAM restorative material surface,
16.17%), and adhesive failures (15.5%) (type 1, com-
plete CAD/CAM restorative material surface was visible)
were also observed. After 30 days of water storage, the
adhesive failure modes increased in the control groups
(Fig 1). Representative SEM images of fractured beams
are presented in Figs 2 and 3.
Two-way ANOVA of the surface roughness testing data
(surface treatment and type of CAD/CAM restorative ma-
terial) revealed that the surface roughness was signifi-
cantly affected by the surface treatment and type of CAD/
CAM restorative material (p < 0.001). There were signifi-
cant interactions between surface treatment and type of
CAD/CAM restorative material (p = 0.006). Means and
standard deviations of the average surface roughness
(Ra, μm) of treated CAD/CAM restorative material with
their significant differences are presented in Table 3. In
general, VE treated with SB showed the significantly high-
est Ra values (4.29 ± 0.34 μm) compared with the other
groups (p < 0.05). Regarding the type of CAD/CAM re-
storative material, LU showed significantly lower Ra values
compared with VE among the groups (p < 0.05) (Table 3).
Representative SEM images of the treated VE and LU
CAD/CAM restorative materials are presented in Figs 4
and 5, respectively. The analysis showed a variation in
the surface microstructures of the VE and LU CAD/CAM
restorative materials with the surface treatments. The
surface topography of untreated VE revealed two con-
tinuous interpenetrating networks: the polymer (dark gray
areas) and the ceramic (light gray areas) with micropores
(Fig 4A). However, the untreated LU showed a more homo-
geneous surface with tiny micropores (Fig 5A).
The surfaces of specimens treated by SB showed well-
defined micro-sized elevated and depressed areas with
crevices and pits which possibly resulted from the high im-
pact of blasting particles (Figs 4B and 5B). VE specimens
treated with HF showed a change in surface texture with
formation of numerous irregular and randomly distributed
gaps and micropores (Fig 4D). HF acid treatment appeared
The Journal of Adhesive Dentistry
 Elsaka

H+S
HF

30 days
SB
+S
Fig 1 Failure pattern dis- SB

LU/BF
tribution of different groups C
tested. Type 1, adhesive fail- H+S
ure: complete CAD/CAM re- HF
storative material surface was SB

24 h
visible. Type 2: mixed failure +S
in CAD/CAM restorative ma- SB
terial surface and luting resin, C
both a part of the CAD/CAM H+S Type 1
restorative material surface HF
Type 2
30 days

and partial luting resin cov- SB

Type 3
erage were visible. Type 3: +S
cohesive failure within the lut- SB Type 4
VE/BF

ing resin layer, almost all of C

the fracture surface was cov- H+S
ered with luting resin. Type 4: HF
mixed failure in CAD/CAM SB
24 h

restorative material surface, +S

luting resin and resin compos- SB
ite, both luting resin and resin C
composite were detected on 0 10 20 30 40 50 60 70 80 90 100
the CAD/CAM restorative ma-
Failure modes (%)
terial surface.

A B C D

C SB SB + S HF
50 μm 50 μm 50 μm

E F G H

HF + S C SB SB + S
50 μm 50 μm 50 μm 50 μm

I J

Fig 2 Representative SEM micrographs (500X) of the

debonded surfaces of the VE/BF system. A−E: after 24 h stor-
age in distilled water; F−J: after 30 days storage in distilled
water. White arrows: retained luting agent; black arrows: VE
restorative material; gray arrow: retained composite. All speci-
mens showed mixed mode of failures except for E and J, which
exhibited cohesive failure within the luting agent, and A and F HF HF + S
with adhesive failure at the interface. 50 μm 50 μm

Vol 16, No 6, 2014 535

Elsaka

A B C D

C SB SB + S HF
50 μm 50 μm 50 μm 50 μm

E F G H

HF + S C SB SB + S
50 μm 50 μm 50 μm 50 μm

I J

Fig 3 Representative SEM micrographs (500X) of the

debonded surfaces of the LU/BF system. A−E: after 24 h
storage in distilled water. F−J: after 30 days storage in dis-
tilled water. White arrows: retained luting agent; black arrows:
LU restorative material; gray arrow: retained composite. All
specimens showed mixed mode of failures except for C, which
HF HF + S showed cohesive failure within the luting agent, and F and I,
50 μm 50 μm with adhesive failure at the interface.

Table 3 Mean (standard deviation) of the average surface roughness values (Ra, μm) of CAD/CAM restorative ma-
terials with different surface treatments

CAD/CAM Surface treatments

restorative material
C SB SB + S HF HF + S
VE 2.21 (0.16)aA 4.29 (0.34)aB 3.91 (0.26)aC 3.77 (0.11)aC 3.29 (0.29)aD

LU 1.12 (0.1)bA 2.73 (0.2)bB 2.57 (0.19)bBC 2.34 (0.22)bCD 2.12 (0.23)bD

Mean values represented with same superscript uppercase letters (row) or lowercase letters (column) are not significantly different according to Tukey’s test
(p > 0.05).

to partially dissolve the polymer and glassy phases of VE, DISCUSSION

which possibly served for micromechanical retention of
resin bonding. However, LU specimens revealed a slight
resistance to HF treatment. Tiny micropores and pits ap-
peared on the LU surface without extensive dissolution of
the glassy phase (Fig 5D). Application of S after SB and
HF surface treatments covered the surface irregularities
created by these treatments and the surface appeared
smoother for both VE (Figs 4C and 4E) and LU (Figs 5C
and 5E).
In recent years, improvements in the adhesion of in-
direct esthetic restorative materials to resin cement
have progressed substantially. Successful adhesion of
indirect restorations to tooth structure can be achieved
by creating a reliable bond between the internal sur-
face of the restoration and the luting agent.37 In this
study, the adhesion of recently introduced VE and LU
CAD/CAM restorative materials to dual-curing self-ad-

536 The Journal of Adhesive Dentistry

 Elsaka

A B C

C SB SB + S
10 μm 10 μm 10 μm

D E

Fig 4 Representative SEM

micrographs (1000X) of VE
specimens after different
surface treatments. White ar-
rows: polymer phase; black HF HF + S
arrow: ceramic phase. 10 μm 10 μm

A B C

C SB SB + S
10 μm 10 μm 10 μm

D E

Fig 5 Representative SEM

micrographs (1000X) of LU
specimens after different sur- HF HF + S
10 μm 10 μm
face treatments.

hesive resin cement after different surface treatments
was determined using the μTBS test. Clinically, indirect
restorations are commonly bonded either to dental tis-
sues or to a core material. In the present study, CAD/
CAM restorative materials were bonded to composite
resin substrates instead of dentin disks. The ration-
ale was to avoid the weak link located in the tooth
structure/luting system interface. The strong bond
developed between composite resin and the luting
system allowed the weak link to be at the CAD/CAM
restorative material/luting system interface. Otherwise,
failures might happen at other sites rather than at the
restorative material surface, thus masking the effects
of the surface treatments.13 In addition, variations in
the tooth microstructure could lead to misinterpreting
the findings.21 Thus, in this study, the CAD/CAM re-
storative material specimens were luted to composite
disks rather to dental substrates.
The μTBS method was chosen as it provides a more
accurate estimation of bond strength compared with

Vol 16, No 6, 2014 537

Elsaka
the conventional shear bond test. The fracture pattern
in shear testing often results in cohesive bulk fracture
within the substrate rather than the interface, due to the
generation of inhomogeneous stress distribution during
testing, which may also lead to invalid interpretation of
the data.1,4,12,14 On the other hand, the μTBS test allows
a more uniform and homogeneous stress distribution
during loading, and failure predominantly occurs at the
adhesive interface due to the small bonded interfaces
(approximately 1 mm2) of the specimens used.1,4,12,14
In addition, the μTBS method enables recognition of the
weakest part in the adhesive system based on the loca-
tion of failure, allowing enhancements to be made to the
relevant part of the adhesive complex.25,36
Selection of the luting agent assumes to be a signifi-
cant factor while bonding to indirect restorations.11,15-17
In the present study, BF dual-curing self-adhesive resin
cement was used as the luting agent to evaluate the
adhesion with VE and LU CAD/CAM restorative materials.
The bond strength of a dual-curing self-adhesive resin
cement with indirect restorations was found to be more
effective than that of a self-curing self-adhesive resin ce-
ment.15,16 This finding was attributed to the acidity of the
adhesive system utilized with the self-curing resin cement,
explained by the presence of non-polymerized residual
acidic monomers in the resinous cement layer. These
residual acidic monomers react with tertiary amines found
in the self-curing resinous cement, neutralizing them; con-
sequently, the tertiary amines are unable to react with
the benzoyl peroxide, which is responsible for the setting
reaction of the polymerization process of this type of ce-
ment.18 Additionally, the self-curing resin cements bond
poorly at the beginning of the luting procedure, meaning
that to avoid dislodgement, the restoration cannot be
subjected to masticatory forces within the first hour.39
Accordingly, microleakage and caries formation could hap-
pen if the restoration is dislodged.6 Hence, dual-curing
resin-based cements are favored as luting materials for
indirect restorations.15,16,39
In this study, the application of HF + S on the bond-
ing surface of VE CAD/CAM restorative material evi-
dently provided higher bond strength compared with
SB and HF surface treatments (Table 2). The HF + S
treatment causes the specimens to fail more in a mixed
mode, often including cohesive failure within the resin
cement (Fig 1). HF surface treatment modifies the mi-
crostructure of the treated surface by partial dissolu-
tion of the glassy or crystalline phases of the restora-
tive material,47 as shown for both VE and LU (Figs 4D
and 5D). HF acid forms microporosities on the restora-
tive material surface, increases the surface area, and
enhances the establishment of mechanical interlocking
with luting resin.34 Roughening the indirect esthetic re-
storative material surface followed by silanization was
anticipated as the preferred technique to achieve a
high bond strength between indirect restorations and
resin-based luting agents.19,30,42 Surface treatment of
VE with SB + S showed comparable bond strength to
HF + S. These findings suggest that surface treatments
of VE restorative material either with HF or SB followed
538
by S application are appropriate treatments. Silane acts
as a coupling agent in the indirect esthetic restorative
material/resin bond, which adsorbs onto the surface of
the restorative material, thus facilitating chemical inter-
action.1 On the other hand, for the LU/BF system, all
surface treatments showed comparable enhancement
of the bond strength values compared with the control
group under different aging periods (Table 2). These
findings suggest that the effect of surface treatment on
the bond strength of resin cement to CAD/CAM restora-
tive is material dependent.
Failure mode analysis supported the results of μTBS
test, as the experimental groups treated with HF  +  S,
SB + S, HF, and SB showed a combination of cohesive
failure in the luting resin and mixed failures, independ-
ent of the type of CAD/CAM restorative material, which
presented with higher bond strength values compared
with the control groups (Fig 1, Table 2). This finding is in
agreement with previous studies.7,31 Cohesive failure of
the luting resin exhibits the perfect bonding status that
can be obtained, as the principal source of failure arises
from flaws within the resin and not at the interface.25,36
In addition, it is noteworthy that the control group, which
had no surface treatment, exhibited more adhesive fail-
ures between the CAD/CAM restorative material and the
luting resin compared with the other groups and showed
significantly lower bond strength values (Fig 1, Table 2).
Mixed and cohesive failure modes are clinically preferable
to total adhesive failure, as the adhesive type of failure
is typically associated with low bond strength values.31,44
This study reveals that the unmodified (untreated) surface
may cause inadequate bonding between the restorative
material and luting agent. Similar findings were reported
previously.14,16
The present study verified the effect of SB and HF
surface treatments on the surface topography of VE and
LU CAD/CAM restorative materials, as shown by surface
roughness and SEM evaluation (Table 3, Figs 4 and 5).
Surface roughness improves mechanical interlocking
with the luting agent, considered as an important fac-
tor that could influence bond strength. SB is anticipated
to enhance the bond strength by improving mechanical
interlocking, increasing wettability and surface area.15,20
However, it was reported in previous studies that SB con-
taminates the indirect esthetic restorative material sur-
face.1,32 In this study, all surface treatments increased
the roughness of VE and LU surface compared with the
control groups (Table 3). Surface roughness should in-
crease surface area and, consequently, may improve the
CAD/CAM restorative material/luting agent bond. For the
groups etched with HF, the surface roughness was lower
than SB treatment; however, the bond strength values of
these groups were comparable to each other (Table 2).
It has been reported that the stress concentration at
the indirect restorative material/luting agent interface
could be increased by airborne-particle abrasion, which
creates sharp angles that could impede complete wetting
and produce voids at the interface.1,32,36 Consequently,
higher surface roughness will not ensure a higher bond
strength.2,7,11,27
The Journal of Adhesive Dentistry

In this study, water storage was used to artificially age
the resin bond for adhesion testing to determine the hy-
drolytic stability of resin cement to CAD/CAM restorative
materials. After 30 days of water storage, the specimens
exhibited significantly lower resin bond strength. This find-
ing could be due to the vulnerability of resin cement to hy-
drolytic degradation, as over time, water absorption at the
interface could reduce the bond strength.41 It has been
reported that the resin cement layer becomes less stiff
over time because of water sorption, which could nega-
tively affect stress distribution across the luted interfaces
to indirect restorations, probably causing debonding even
under weak occlusal loads.45 This finding is in agreement
with previous studies.5,31,36,41 It is noteworthy that after
aging, the VE/BF system showed higher bond strength
values compared with the LU/BF system (Table 2). This
finding indicates that the bond strength of the VE/BF sys-
tem appears to be more hydrolytically stable and durable
than the LU/BF system, even with a significant decrease
in bond strength values after aging. In addition, the bond
strength for the VE/BF system was statistically signifi-
cantly higher than for the LU/BF system in all groups,
regardless of the surface treatment (Table 2). This find-
ing could be attributed to the different composition and
microstructure between VE and LU. The microstructure
of VE is comprised of a feldspar ceramic network that
is fully integrated with a polymer network. VE presented
with a low polymer content (14 wt%). This microstruc-
ture could have a significant influence on the mechanical
properties, such as increased chemical stability, reduced
monomer absorption, and greater biocompatibility. It has
been claimed that the strength and elasticity of the PICN
restorative material could provide a highly fracture-resist-
ant material.10,23,38,43,46 It has also been reported that
VE could withstand high levels of elongation at high stress
before fracturing, due to the integrated polymer network
that facilitates high levels of stability, in spite of a lower
modulus of elasticity.43 It has been supposed that en-
tirely merging the networks with each other like this also
provides integrated crack prevention as well as creating a
structure that offers greater fault tolerance.10,23,43,46 On
the other hand, regarding the microstructure of LU, it is a
polymer network (20 wt%) reinforced by 80 wt% zirconia/
silica nanoceramic particles.28 It could be postulated that
LU showed lower adhesion values with BF luting agent
compared with VE due to the differences in the micro-
structures, composition, filler type, filler concentration,
and mechanical properties of the two tested CAD/CAM re-
storative materials. It is noteworthy that the surface treat-
ments performed also enhanced the adhesion of LU with
BF luting resin compared with the control group (Table 2).
CONCLUSIONS
Based on the results presented and within the limita-
tions of this study, it can be concluded that the effect of
surface treatments on the bond strength of novel CAD/
CAM restorative materials to resin cement is material
dependent. The VE/BF system revealed higher bond
Vol 16, No 6, 2014
Elsaka
strength than the LU/BF system. Water aging showed
a considerable influence on restorative material/luting
resin bond degradation. The VE/BF system appears
to be more hydrolytically stable and durable than the
LU/BF system. Further research is needed to evaluate
the physical properties of the novel CAD/CAM restora-
tive materials VE and LU to clarify their behavior. Such
evaluations might lead to a better understanding of the
behavior of these materials. Future studies are also re-
quired on the participation of the tooth substrates in the
test complex under standardized conditions. Only one
brand of resin cement was tested in this study; the find-
ings related to this product may not be valid for other,
similar materials. Additionally, evaluation of the clinical
performance is required to provide reliable recommenda-
tions for dental practitioners.
ACKNOWLEDGMENTS
The author would like to thank VOCO, Vita Zahnfabrik, and Ultra-
dent for supplying the materials for this research.
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Clinical relevance: The VE/BF system provided
higher bond strength than the LU/BF system under
different aging periods. The influence of surface treat-
ments on the bond strength was more effective on
the VE CAD/CAM restorative material than on the LU
material.
The Journal of Adhesive Dentistry
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