Influence of Pretreatment Methods on the Adhesion of

Composite and Polymer Infiltrated Ceramic CAD-CAM Blocks

Isabel Emsermanna / Florin Eggmannb / Gabriel Krastlc / Roland Weigerd / Julia Amatoe

Purpose: To assess the effect of different surface pretreatments on the shear bond strength of resin luting material
on CAD-CAM composite resins and a polymer-infiltrated ceramic network (PICN).
Materials and Methods: CAD-CAM materials (Brilliant Crios, Cerasmart, Lava Ultimate, VITA Enamic) were sub-
jected to the following pretreatments: no pretreatment; grit blasting; grit blasting + silane; HF etching + silane; tri-
bochemical silica coating + silane; manufacturers’ specifications; manufacturers’ specifications + silane;
manufacturers’ specifications using only the manufacturers’ products including their recommended luting materials
(DuoCem, G-Cem LinkForce, RelyX Ultimate, RelyX Unicem 2). Specimens were luted with resin luting material ac-
cording to the Swiss shear test design. After six months of water storage, shear bond tests were performed. Data
were analyzed with multiple linear regression models and nested models (α = 0.05).
Results: Low bond strengths were obtained without pretreatment (Brilliant Crios 3.01 ± 0.54 MPa, Cerasmart
2.66 ± 0.47 MPa, Lava Ultimate 1.76 ± 0.26 MPa, VITA Enamic 2.83 ± 0.63 MPa). Grit blasting achieved high
bond strengths across all materials (Brilliant Crios 5.17 ± 0.77 MPa, Cerasmart 4.27 ± 0.50 MPa, Lava Ultimate
3.98 ± 0.54 MPa, VITA Enamic 4.97 ± 0.90 MPa). Silane application tended to decrease bond strengths on CAD-
CAM composite resins. Following the manufacturers’ specifications and using their recommended materials
achieved the highest bond strengths for all materials except Cerasmart (Brilliant Crios 5.75 ± 0.91 MPa,
Cerasmart 2.82 ± 0.28 MPa, Lava Ultimate 6.63 ± 0.97 MPa, VITA Enamic 7.09 ± 0.77 MPa).
Conclusion: Grit blasting and the application of a suitable material primer is a useful pretreatment for the bonding
of CAD-CAM composite resins. Silane application on CAD-CAM composite resins may entail drawbacks, possibly
owing to the scarcity of silanizable fillers.
Keywords: silane primer, hydrofluoric acid etching, silica coating, air abrasion, adhesion.

J Adhes Dent 2019; 21: 433–443. Submitted for publication: 15.01.19; accepted for publication: 14.07.19
doi: 10.3290/j.jad.a43179

N owadays it is commonplace to use computer-aided de-

sign and computer-aided manufacturing (CAD-CAM) to
fabricate indirect restorations. An extensive range of mater-
ials is currently available for CAD-CAM restorations.32
CAD-CAM composite resins with dispersed fillers and VITA
Enamic (VITA Zahnfabrik; Bad Säckingen, Germany), a PICN
(polymer-infiltrated ceramic network) material also termed
hybrid ceramic, were introduced on the dental market re-
cently.35
CAD-CAM composite resins consist of a polymeric matrix
and dispersed fillers. The fillers can be organic, inorganic
(ie, ceramics, glass-ceramics, or glasses), or composite.2,18
VITA Enamic, on the other hand, consists of two continuous
interconnected networks, one feldspathic ceramic (86 wt%)

a Resident, Department of Periodontology, Endodontology and Cariology, Uni-
versity Center for Dental Medicine, University of Basel, Basel, Switzerland. Ex-
perimental design, performed the experiments, contributed substantially to
discussion, wrote the manuscript, with Florin Eggmann contributed equally to
this work.
b Resident, Department of Periodontology, Endodontology and Cariology, Uni-
versity Center for Dental Medicine, University of Basel, Basel, Switzerland. Ex-
perimental design, contributed substantially to discussion, wrote the
manuscript, with Isabel Emsermann contributed equally to this work.
c Professor and Director, Department of Operative Dentistry and Periodontol-
ogy, Julius Maximillians University of Würzburg, Würzburg, Germany. Research
idea, experimental design, contributed substantially to discussion, proofread
the manuscript.
d Professor and Director, Department of Periodontology, Endodontology and
Cariology, University Center for Dental Medicine, University of Basel, Basel,
Switzerland. Research idea, contributed substantially to discussion, proofread
the manuscript.
e Head of Division of Cariology, Department of Periodontology, Endodontology
and Cariology, University Center for Dental Medicine, University of Basel,
Basel, Switzerland. Research idea, experimental design, contributed substan-
tially to discussion, proofread the manuscript.
Correspondence: Dr. med. dent. Florin Eggmann, Department of Periodontology,
Endodontology and Cariology, University Center for Dental Medicine, University
of Basel, Mattenstrasse 40, CH-4058 Basel, Switzerland. Tel. +41-61-267-2680;
email: florin.eggmann@unibas.ch

Vol 21, No 5, 2019 433

Emsermann et al
and one polymeric (14 wt%).14,32 The hardness, flexural
strength, and flexural modulus of CAD-CAM composite res-
ins and VITA Enamic are significantly lower than those of
ceramic materials.2,32
No long-term data on the clinical performance of VITA
Enamic are available at present. Promising survival rates in
the range of 95.6% to 97% have been reported for PICN in-
lays, partial coverage restorations, and crowns inserted with
resin luting material after observation periods of up to three
years.5,17,34 Clinical evidence demonstrates, however, that
PICN restorations are prone to debonding if the luting proto-
col is not in accordance with the material-specific recom-
mendations.5 Likewise, no long term clinical data are cur-
rently available for CAD-CAM composite resin restorations.
A preliminary clinical study with an observation period of
two years reported a survival rate of 85.7% and a debond-
ing rate of 7.1% for partial coverage restorations made with
CAD-CAM composite resin.44 The existing body of clinical
evidence suggests an increased susceptibility to bonding
failure, and it indicates that the adhesive performance of
restorations made with CAD-CAM composite resins and the
PICN material is highly dependent on the bonding protocol.
The pretreatment and bonding protocol needs to be tai-
lored to the microstructural characteristics of CAD-CAM ma-
terials.31 The degree of conversion of CAD-CAM composite
resins substantially exceeds that of conventional filling
composite resins. The industrial polymerization mode of
CAD-CAM composite resins can increase the degree of con-
version up to 96% and it also rises the crosslink density.10
As a consequence, few free monomers remain available for
copolymerization with monomers of the resin luting mater-
ial.10 The scarcity of unreacted monomers requires that
surface pretreatment and bonding approach be adapted,
434
Fig 1 Overview of the
study design (modified
from Lise et al16). GB: grit
blasting; HF: hydrofluoric
acid etching; RXU: RelyX
Unicem 2; SC: tribo-
chemical silica-coating
with CoJet; SI: silane
application.
because micromechanical interlocking is crucial for the per-
formance of the adhesive interface.10
However, in contrast to glass ceramics, the surface pre-
treatment and bonding protocols that are best suited for
different CAD-CAM composite resins and PICN materials
have not yet been conclusively determined.25 There is, for
instance, conflicting data on the efficacy of silane coupling
agents as material primers for CAD-CAM composite res-
ins.8,23 Furthermore, the surface pretreatment methods
and materials that are recommended by the manufacturers
show considerable differences.
Thus, the aim of this in vitro study was to evaluate the
effect of different surface pretreatment protocols for CAD-
CAM composite resins and a PICN material on the shear
bond strength of resin luting material. The study assessed
the adhesive impact of different standard surface pretreat-
ments, namely, grit blasting, tribochemical silicia-coating,
and HF etching, as well as silane primer application. More-
over, the pretreatment methods recommended by the man-
ufacturers of the CAD-CAM materials, both with generic lut-
ing agents and their recommended resin luting materials,
were compared with these standard surface pretreatment
protocols. The null hypothesis tested was that there would
be no difference between the shear bond strengths of the
different surface pretreatment groups.
MATERIALS AND METHODS
Sample Preparation and Surface Pretreatment
The experimental procedure is outlined in Fig 1. The investiga-
tion included three CAD-CAM composite resins, Brilliant Crios
(Coltène/Whaledent; Altstätten, Switzerland), Cerasmart (GC
The Journal of Adhesive Dentistry

Europe; Leuven, Belgium), Lava Ultimate (3M Oral Care, St
Paul, MN, USA), and a CAD-CAM PICN material, VITA Enamic
(VITA Zahnfabrik; Bad Säckingen, Germany). Table 1 lists the
manufacturers and compositions of the materials used.
CAD-CAM blocks (size 14) were cut under constant water
cooling with a semi-automated diamond-blade saw
(Exakt30/700, Exakt Advanced Technologies; Norderstedt,
Germany) into four 4-mm-thick slabs. To achieve surface
roughness comparable to that obtained through CAD-CAM
milling, the slabs were wet ground with 180-grit Al2O3-
paper (Reflex NAC Type S P180, Presi; Eybens, France)
for 20 s. This grinding procedure was based on unpub-
lished data from preliminary profilometrical tests (Hommel
Tester T1000, TKK 50, Hommel-Etamic; Villingen-
Schwenningen, Germany) that determined the surface
roughness of every tested CAD-CAM material after pro-
cessing in a milling and grinding unit (Cerec MC XL,
Dentsply Sirona; Bensheim, Germany). All slabs were ul-
trasonically cleaned in three alternating solutions (distilled
water, ethanol [96%], distilled water), each for 180 s, to
remove surface contaminants.
In groups G1-NO, G2-GB, G3-GB-SI, G4-HF-SI, and G5-SC-
SI (details given below), simplified standard protocols were
tested to assess whether simplified surface pretreatment
protocols achieve favorable bond strengths. The surface
pretreatments were identical for all CAD-CAM materials
within each group. In contrast, groups G6-MS, G7-MS-SI,
and G8-MS-MP (details given below) followed the recom-
mended manufacturers’ specifications. The surface pre-
treatments within those groups differed as the manufactur-
ers’ specifications were distinctly different.
In the seven groups G1-NO through to G7-MS+SI, RelyX
Unicem 2 Clicker (3M Oral Care) was used as self-adhesive
resin luting material, whereas in G8-MS-MP the respective
resin luting materials recommended by the manufacturers
were used.
The slabs of each material were randomly divided into 8
groups (n = 20) and subjected to the following 8 surface
pretreatments.
G1-NO: no surface pretreatment.
G2-GB: grit blasting. The surface was grit blasted with 50-μm
aluminum oxide particles (Renfert; Hilzingen, Germany) per-
pendicular to the surface from a distance of 10 mm for 5 s
at a pressure of 0.15 MPa. The surface was thoroughly
rinsed with water spray for 10 s and air blown for 5 s.
G3-GB-SI: grit blasting + silane. The surface was grit
blasted following the same protocol as in G2-GB. Thereafter
silane (Ultradent Silane, Ultradent; South Jordan, UT, USA)
was brushed onto the surface for 60 s using a disposable
microtip applicator. After 60 s, the surface was dried by
gentle air blowing for 5 s.
G4-HF-SI: HF etching + silane. The surface was etched with
5% HF (Vita Ceramics Etch, Vita Zahnfabrik) for 60 s, thor-
oughly rinsed with water spray for 10 s, and dried by air
Vol 21, No 5, 2019
Emsermann et al
blowing for 5 s. Thereafter, silane (Ultradent Silane, Ultra-
dent) was brushed onto the surface for 60 s using a dispos-
able microtip applicator. After 60 s, the surface was dried
by gentle air blowing for 5 s.
G5-SC-SI: tribochemical silica-coating + silane. The surface
was grit blasted with 30 μm CoJet particles (3M Oral Care)
perpendicular to the surface from a distance of 10 mm for
5 s at a pressure of 0.2 MPa. The surface was thoroughly
rinsed by water spray for 10 s and air blown for 5 s. Thereaf-
ter, silane (Ultradent Silane, Ultradent) was brushed onto the
surface for 60 s using a disposable microtip applicator. After
60 s, the surface was dried by gentle air blowing for 5 s.
G6-MS: manufacturers’ specifications
y Brilliant Crios: grit blasting + One Coat 7 Universal
(Coltène/Whaledent). The surface was grit blasted fol-
lowing the same protocol as in G2-GB, then One Coat 7
Universal (Coltène/Whaledent) was applied onto the sur-
face for 20 s using a disposable microtip applicator and
air blown for 5 s.
y Cerasmart: the manufacturer’s specifications were iden-
tical to G3-GB-SI. Therefore, the values obtained in G3-
GB-SI were used for the statistical analysis.
y Lava Ultimate: tribochemical silica-coating + Scotchbond
Universal (3M Oral Care). The surface was grit blasted
with 30-μm CoJet particles (3M Oral Care) perpendicular
to the surface from a distance of 10 mm for 5 s at a
pressure of 0.2 MPa. The surface was thoroughly rinsed
with water spray for 10 s and air blown for 5 s. Then
Scotchbond Universal (3M Oral Care) was applied onto
the surface for 20 s using a disposable microtip applica-
tor and the surface was air blown for 5 s.
y VITA Enamic: the manufacturer’s specifications were
identical to G4-HF-SI. Therefore, the values obtained in
G4-HF-SI were used for the statistical analysis.
G7-MS-SI: manufacturers’ specifications + silane
y Brilliant Crios: The surface was grit blasted with 50 μm
aluminum oxide particles (Renfert) perpendicular to the
surface from a distance of 10 mm for 5 s at a pressure
of 0.15 MPa. The surface was thoroughly rinsed by water
spray for 10 s and air blown for 5 s. Thereafter, silane
(Ultradent Silane) was brushed onto the surface for 60 s
using a disposable microtip applicator. After 60 s, the
surface was dried with a gentle air stream for 5 s. Then
One Coat 7 Universal (Coltène/Whaledent) was applied
onto the surface for 20 s using a disposable microtip
applicator and air blown for 5 s.
y Cerasmart: the manufacturer’s specifications were iden-
tical to G3-GB-SI. Therefore, the values obtained in G3-
GB-SI were used for the statistical analysis.
y Lava Ultimate: The surface was grit blasted with 30 μm
CoJet particles (3M Oral Care) perpendicular to the sur-
face from a distance of 10 mm for 5 s at a pressure of
0.2 MPa. The surface was thoroughly rinsed by water
spray for 10 s and air blown for 5 s. Thereafter, silane
(Ultradent Silane) was brushed onto the surface for 60 s
435
Emsermann et al

Table 1 General composition of materials tested in this study

Materials Composition Batch No.

CAD-CAM Brilliant Crios Inorganic portion (71 wt%): amorphous silicia SiO2 (<20 nm), barium glass I16275
composite (Coltène/Whaledent; (<1 μm)
resin Altstätten,
Switzerland) Polymers (29 wt%): cross-linked methacrylates bis-GMA, bis-EMA, TEG-DMA

CAD-CAM Cerasmart (GC Inorganic portion (71 wt%): silica SiO2 (20 nm) and barium glass (300 nm) 1707251
composite Europe ; Leuven, nanoparticles
resin Belgium)
Polymers (29 wt%): bis-MEPP, UDMA, DMA

CAD-CAM Lava Ultimate (3M Inorganic portion (80 wt%): 69% SiO2 (20nm), 31% ZrO2 (4-11nm) particles and N895353
composite Oral Care; St Paul, aggregated ZiO2/SiO2 nanoclusters (0.6-10 μm)
resin MN, USA)
Polymers (20 wt%): bis-GMA, UDMA, bis-EMA, TEG-DMA

CAD-CAM VITA Enamic (VITA Inorganic portion (86 wt%): SiO2 (20 nm), ZrO2 (4–11 nm), aggregated ZrO2/SiO2 61011
PICN material Zahnfabrik; Bad cluster
Säckingen, Germany)
Polymers (14 wt%): UDMA, TEG-DMA

Conventional DuoCem (Coltène/ Base/catalyst: bis-GMA 10-<15%, TEG-DMA 5-<10%, zinc oxide coated 1-<5%, H96929
resin luting Whaledent) dibenzoyl peroxide <1%, sodium fluoride <1%
material

Conventional G-Cem LinkForce (GC Base paste: UDMA 20-25%, dimethacrylate 5-10%, stabilizer <0.5% 1703231
resin luting Europe)
material Catalyst paste: UDMA 20-25%, bis-EMA 5-10%, dibenzoyl peroxide <1%, butylated
hydroxytoluene <0.5%

Conventional RelyX Ultimate (3M Base paste: methacrylate monomers, radiopaque silanated fillers, initiator 3402147
resin luting Oral Care) components, stabilizers, rheological additives
material Catalyst paste: methacrylate monomers, radiopaque alkaline (basic) fillers,
initiators components, stabilizers, pigments, rheological additives, fluorescence
dye, dark cure activator for Scotchbond Universal

Self-adhesive RelyX Unicem 2 Base paste: methacrylate monomers containing phosphoric acid groups, 3362211
resin luting Clicker (3M Oral methacrylate monomers, silanated fillers, initiator, stabilizers
material Care)
Catalyst paste: methacrylate monomers, alkaline (basic) fillers, initiators
components, stabilizers, pigments

Grit-blasting Aluminum oxide 50 μm alumina particles: 99.7% Al2O3, SiO2 <0.02% 3022554
particles (Renfert; Hilzingen,
Germany)

Grit-blasting CoJet (3M Oral Care) 30 μm alumina particles modified by silica (Al2O3 >97%, silica <3%) 3454446
particles

Hydrofluoric Vita Ceramics Etch ≤ 5% hydrofluoric acid and ≤ 10% sulfuric acid, ethanol 54330
acid (VITA Zahnfabrik)

Silane primer G-Multi Primer (GC Ethyl alcohol 90-100%, 2,2’-ethylenedioxydiethyl dimethacrylate 1-<2.5%, 1703231
Europe)
(1-methylethylidene)bis[4,1-phenyleneoxy(2-hydroxy-3,1-propanediyl)]
bismethacrylate, 3-trimethoxysilylpropyl methacrylate

Silane primer Ultradent Silane Methacryloxypropyltrimethoxy silane < 10%, isopropyl alcohol < 95% 366177
(Ultradent; South
Jordan, UT, USA)

Silane primer Vitasil (VITA 3-trimethoxysilylpropyl methacrylate <2.5%, ethanol 25-50% 57620
Zahnfabrik)

Universal One Coat 7 Ethanol 35- <40%, UDMA 20- <25%, HEMA 5- < 10%, MMA-modified polyacrylic I09273
adhesive (Coltène/Whaledent) acid, hydroxypropylmethacrylate

Universal Scotchbond 10-MDP 1-10%, dimethacrylate resins 5-15%, HEMA 15-25%, Vitrebond copolymer 70822A
adhesive Universal (3M Oral 1-10%, filler, ethanol 10-15%, water, initiators, silane 5-15%
Care)

Bis-GMA (2,2-bis[4-(2-hydroxy-3-methacryloxypropoxy)phenyl]propane), UDMA (urethane dimethacrylate), MMA (methyl-methacrylate), bis-EMA (2,2-bis[4-methac-

ryloxypolyethoxyphenyl)propane]), TEG-DMA (triethylene glycol dimethacrylate), DMA (dodecyl dimethacrylate, HEMA (2-hydroxyethyl methacrylate), 10-MDP(10-
methacryloyloxydecyl dihydrogen phosphate).

436 The Journal of Adhesive Dentistry


using a disposable microtip applicator. After 60 s, the
surface was dried with a gentle air stream for 5 s.
Scotchbond Universal (3M Oral Care) was applied onto
the surface for 20 s using a disposable microtip applica-
tor and the surface was air blown for 5 s.
y VITA Enamic: the manufacturer’s specifications were
identical to G4-HF-SI. Therefore the values obtained in
G4-HF-SI were used for the statistical analysis.
G8-MS-MP: using only the manufacturers’ products and
the recommended resin luting materials
y Brilliant Crios: the surface was treated following the
same protocol as in G6-MS and DuoCem (Coltène/Whale-
dent) was used as conventional resin luting material.
y Cerasmart: the surface was grit blasted following the
same protocol as in G2-GB, then silane (GC-Primer, GC
Europe) was applied onto the surface for 20 s using a
disposable microtip applicator and dried with a gentle air
stream for 5 s. G-Cem Link Force (GC Europe) was used
as conventional resin luting material.
y Lava Ultimate: the surface was treated following the
same protocol as in group 6 (G6-MS) and RelyX Ultimate
(3M Oral Care) was used as conventional resin luting
material.
y VITA Enamic: the surface was etched with 5% HF (Vita
Zahnfabrik) for 60 s, thoroughly rinsed by water spray for
10 s and dried with an air stream for 5 s. Then silane
(Vitasil, Vita Zahnfabrik) was applied onto the surface for
20 s using a disposable microtip applicator and allowed
to react for 5 min. Subsequently, Rely X Unicem 2 Clicker
(3M Oral Care) was used as resin luting material.
Swiss Shear Test Design
The procedure of the Swiss shear test has been described
in detail elsewhere.1,36 In brief, after surface pretreatment,
a hollow cylinder of clear acrylic with an internal diameter of
2.9 mm and a height of 4 mm (D+R Tec; Birmensdorf, Swit-
zerland) was attached to the surface using a custom-made
bonding jig. The resin luting material, mixed according to
the manufacturers’ instructions in mixing syringe dispens-
ers, was applied into this cylinder and a stainless steel bolt
with a diameter matching the hollow cylinder (Bossard; Zug,
Switzerland) was inserted in the cylinder. The bolt was
loaded with 1 kg with the help of the bonding jig to spread
the resin luting material evenly on the substrate surface
without entrapping air. The resin luting material was light
cured from three different sides for 20 s per side at an out-
put intensity of 1200 mW/cm2 (high-power mode, Blue-
phase 20i, Ivoclar Vivadent; Schaan, Liechtenstein). Imme-
diately after the bonding procedure, the specimens were
removed from the bonding jig, placed in demineralized water
at 37°C, and stored for 6 months under these conditions.
Shear Test and Failure Type Analysis
After water storage for 6 months, shear bond strength tests
were performed with a universal testing machine (Zwick/
Roell; Ulm, Germany) at a crosshead speed of 1 mm/min.
The machine applied the load onto the acrylic hollow cylin-
Vol 21, No 5, 2019
Emsermann et al
der at a distance of 2 mm from the adhesive surface until
fracture occurred. Shear bond strengths, recorded in MPa,
were calculated by dividing the maximum load at failure (N)
with the cross-sectional area (mm2).
The failure modes were assessed under a light micro-
scope (Leica M7A, Leica Microsystems; Wetzlar, Germany)
at a magnification of 31X. Failures were classified as adhe-
sive (shear fracture between the luting agent and the CAD-
CAM material), cohesive type 1 (shear fracture within the
luting agent), cohesive type 2 (shear fracture within the
CAD-CAM material), or mixed failures (involvement of adhe-
sive and both types of cohesive fractures).
Statistical Analysis
A statistician carried out the statistical analyses with R soft-
ware (version 3.1.2., R Core Team, R Foundation for Statis-
tical Computing; Vienna, Austria). Descriptive statistics in-
cluded means and standard deviations (SD). Multiple linear
regression models were performed to compare shear bond
strengths between the pretreatment groups. Nested model
designs were chosen to accommodate all possible com-
parisons. Differences of mean values were estimated to-
gether with 95% confidence intervals and the corresponding
p-values. The level of significance, unadjusted for multiple
comparisons, was set at 5%.
RESULTS
No pre-test failures occurred during water storage. Owing to
failures in technical handling (partial damage during mount-
ing specimens in the testing machine), 24 out of 560 spec-
imens were excluded from data analysis. Surface pretreat-
ment had a significant effect on bond strengths across all
CAD-CAM materials tested (p < 0.001). The mean shear
bond strengths are listed in Table 2. Table 3 shows the re-
sults of the multiple linear regressions. For all materials,
bond strengths were significantly higher when grit blasting
was performed compared with no surface pretreatment
(p < 0.001). Surface pretreatment according to the manu-
facturers’ specifications (G6-MS) yielded significantly higher
bond strengths than did HF etching and subsequent silane
application (G4-HF-SI) on CAD-CAM composite resins
(p < 0.001). The comparison between grit blasting + silane
application (G3-GB-SI) and HF etching + silane application
(G4-HF-SI) showed no significant difference for Lava Ulti-
mate (p = 0.250), significantly higher bond strengths for
VITA Enamic in G4-HF-SI (p = 0.003), and superior bond
strengths for Brilliant Crios and Cerasmart in G3-GB-SI
(p = 0.005 and p < 0.001, respectively). For the CAD-CAM
composite resins whose manufacturers do not recommend
an additional surface pretreatment step of silane (ie, Bril-
liant Crios and Lava Ultimate), silanization in addition to the
recommended protocol had no significant effect on bond
strength (p ≥ 0.056). No significant differences were ob-
served between grit blasting + silane application (G3-GB-SI)
and tribochemical silica coating + silane application (G5-SC-
SI) for all materials (p ≥ 0.238) apart from Cerasmart,
437
Emsermann et al

Table 2 Means and standard deviations (SD) of the shear bond strengths (MPa) after different surface pretreatments

Material G1-NO G2-GB G3-GB-SI G4-HF-SI G5-SC-SI G6-MS G7-MS-SI G8-MS-MP

Brilliant 3.01 (0.54)B 5.17 (0.77)C 2.51 (0.89)B 1.79 (0.55)A 2.82 (1.11)B 5.32 (0.56)CD 5.80 (0.78)D 5.75 (0.91)D
Crios
n = 19 n = 20 n = 19 n = 19 n = 18 n = 20 n = 20 n = 20

Cerasmart 2.66 (0.47)C 4.27 (0.50)D 2.94 (0.81)C 1.63 (0.50)A 2.24 (0.94)B 2.94 (0.81)C 2.94 (0.81)C 2.82 (0.28)C

n = 20 n = 20 n = 20 n = 18 n = 18 n = 20 n = 20 n = 20

Lava 1.76 (0.26)A 3.98 (0.54)B 2.14 (0.54)A 1.82 (0.50)A 1.82 (0.75)A 6.41 (0.87)C 6.59 (0.90)C 6.63 (0.97)C
Ultimate
n = 19 n = 20 n = 18 n = 17 n = 18 n = 20 n = 19 n = 20

VITA 2.83 (0.63)A 4.97 (0.90)C 2.82 (1.08)A 3.63 (1.54)B 2.96 (1.18)A 3.63 (1.54)B 3.63 (1.54)B 7.10 (0.77)D
Enamic
n = 20 n = 20 n = 18 n = 18 n = 18 n = 18 n = 18 n = 20

Different superscript upper case letters indicate statistically significant differences within each row.

which showed significantly higher bond strengths in G3-GB-
SI (p = 0.007). For Cerasmart and VITA Enamic, grit blast-
ing (G2-GB) resulted in significantly higher bond strengths
than surface pretreatment according to the manufacturers’
recommendations (G6-MS) (p < 0.001). No significant dif-
ference between G6-MS and G2-GB was found for Brilliant
Crios (p = 0.540) while for Lava Ultimate, surface pretreat-
ment according to the manufacturer’s recommendations
(G6-MS) resulted in significantly higher bond strengths than
grit blasting (G2-GB) (p < 0.001). Surface pretreatment ac-
cording to the manufacturers’ recommendations (G6-MS)
obtained significantly higher bond strengths than grit blast-
ing and silane application (G3-GB-SI) for Brilliant Crios
(p < 0.001), VITA Enamic (p = 0.003), and Lava Ultimate
(p < 0.001). For Brilliant Crios, Cerasmart, and Lava Ulti-
mate, surface pretreatment according to the manufacturers’
recommendations in combination with their recommended
resin luting materials (G8-MS-MP) was not significantly dif-
ferent from surface pretreatment according to the manufac-
turers’ recommendations without using their recommended
resin luting materials (G6-MS) (p = 0.088, p = 0.658, and
p = 0.378, respectively). For VITA Enamic, a statistically sig-
nificant difference was recorded between G8-MS-MP and all
the other groups (p < 0.001); ie, the surface pretreatment
according to the manufacturer’s recommendation combined
with the recommended materials showed the highest bond
strengths. Grit blasting (G2-GB) was the best performing
surface pretreatment for Cerasmart; surface pretreatment
according to the manufacturer’s recommendation resulted
in significantly lower bond strength (p < 0.001).
Table 4 presents the results from the failure mode
analysis. In the absence of any surface pretreatment, all
specimens showed adhesive failure. Adhesive failure was
most frequently observed for Brilliant Crios in groups G2-GB
to G6-MS, while in G7-MS-SI and G8-MS-MP, adhesive and
mixed failures were more uniformly distributed. When the
surface of Cerasmart was not treated with grit blasting, ad-
hesive failure was most common. The most frequent failure
mode for VITA Enamic was cohesive within the resin luting
material in G8-MS-MP. For Lava Ultimate, the specimens
fractured most commonly within the CAD-CAM composite
resin when Scotchbond Universal was used as surface pre-
treatment (G6-MS, G7-MS-SI, G8-MS-MP), otherwise adhe-
sive failures prevailed.
DISCUSSION
This in vitro study assessed the effect of different surface
pretreatment protocols on the bond strength of resin luting
material to CAD-CAM composite resins and a PICN material.
The results showed that following the surface pretreatment
protocols recommended by manufacturers yielded the high-
est bond strengths for the PICN material and all CAD-CAM
composite resins, apart from Cerasmart. Application of a
silane coupling agent tended to decrease bond strength to
CAD-CAM composite resins.
High bond strengths to the CAD-CAM materials were
achieved in the present study when the surface was grit
blasted at a pressure of 0.15 MPa. This is in close agree-
ment with previous studies and evidence-based recommen-
dations.22,25 The present study focused solely on bond
strength, but it is also important to consider that high-pres-
sure grit blasting can damage CAD-CAM composite res-
ins.38,41 There are recommendations underpinned by la-
boratory evidence for different CAD-CAM composite resins
concerning particle size and pressure, and it is advisable to
follow these recommendations in clinical practice.38 If air-
borne-particle abrasion is chosen as the surface pretreat-
ment for VITA Enamic with its feldspathic ceramic structure
network, grit blasting should be performed with due care.
The use of small particles and low pressures is of particular
importance, because otherwise surface damage and crack
formation may occur.38 Moreover, it is important to note
that the intraoral repair of indirect composite resin and ce-
ramic restorations constitutes an indication for grit blasting.

438 The Journal of Adhesive Dentistry

 Emsermann et al

Table 3 Results of the multiple linear regressions with a nested model design

Difference of
Comparison between groups Material 95% CI p-value
means
G2-GB vs G1-NO Brilliant Crios 2.16 1.66 2.66 < 0.001
G2-GB vs G1-NO Cerasmart 1.61 1.12 2.10 < 0.001
G2-GB vs G1-NO Lava Ultimate 2.22 1.72 2.73 < 0.001
G2-GB vs G1-NO VITA Enamic 2.14 1.65 2.64 < 0.001
G3-GB-SI vs G4-HF-SI Brilliant Crios 0.72 0.22 1.23 0.005
G3-GB-SI vs G4-HF-SI Cerasmart 1.31 0.80 1.82 < 0.001
G3-GB-SI vs G4-HF-SI Lava Ultimate 0.31 -0.22 0.84 0.250
G3-GB-SI vs G4-HF-SI VITA Enamic -0.81 -1.33 -0.29 0.003
G3-GB-SI vs G5-SC-SI Brilliant Crios -0.31 -0.82 0.21 0.245
G3-GB-SI vs G5-SC-SI Cerasmart 0.70 0.19 1.21 0.007
G3-GB-SI vs G5-SC-SI Lava Ultimate 0.31 -0.21 0.84 0.238
G3-GB-SI vs G5-SC-SI VITA Enamic -0.13 -0.66 0.39 0.616
G6-MS vs G2-GB Brilliant Crios 0.16 -0.34 0.65 0.540
G6-MS vs G2-GB Cerasmart -1.34 -1.83 -0.84 < 0.001
G6-MS vs G2-GB Lava Ultimate 2.43 1.93 2.92 < 0.001
G6-MS vs G2-GB VITA Enamic -1.34 -1.85 -0.84 < 0.001
G6-MS vs G3-GB-SI Brilliant Crios 2.81 2.31 3.31 < 0.001
G6-MS vs G3-GB-Si Cerasmart – – – –
G6-MS vs G3-GB-SI Lava Ultimate 4.27 3.76 4.78 < 0.001
G6-MS vs G3-GB-SI VITA Enamic 0.81 0.29 1.33 0.003
G6-MS vs G4-HF+SI Brilliant Crios 3.53 3.03 4.04 < 0.001
G6-MS vs G4-HF+SI Cerasmart 1.31 0.80 1.82 < 0.001
G6-MS vs G4-HF+SI Lava Ultimate 4.58 4.06 5.10 < 0.001
G6-MS vs G4-HF-Si VITA Enamic – – – –
G6-MS vs G7-MS-SI Brilliant Crios -0.48 -0.98 0.01 0.056
G6-MS vs G7-MS-SI Cerasmart – – – –
G6-MS vs G7-MS-SI Lava Ultimate -0.18 -0.68 0.32 0.476
G6-MS vs G7-MS-SI VITA Enamic – – – –
G6-MS vs G8-MS-MP Brilliant Crios -0.43 -0.93 0.07 0.088
G6-MS vs G8-MS-MP Cerasmart 0.11 -0.38 0.61 0.650
G6-MS vs G8-MS-MP Lava Ultimate -0.22 -0.72 0.27 0.378
G6-MS vs G8-MS-MP VITA Enamic -3.46 -3.97 -2.96 < 0.001

Compared with grit blasting, tribochemical silica-coating
did not improve the adhesive performance in the present
study; in fact, for one CAD-CAM composite resin, it even
decreased the bond strength. A more relevant influence on
bond strength has been attributed to different particle sizes
than to their chemical composition.24 Grit blasting was per-
formed with aluminum oxide particles with a size of 50 μm.
CoJet sand, by comparison, has a finer particle size of
about 30 μm and consequently a lower abrasion rate. This
may explain the results of the present study, which, in ac-
cordance with previous investigations, suggest that micro-
mechanical conditioning is the key step for adequate adhe-
sion to CAD-CAM composite resins.7,23
HF etching leads to lower bond strengths than grit blast-
ing for most composite resins.18 In the present study, the
adhesive performance on all CAD-CAM composite resins
was better with the grit blasting pretreatment than with HF
etching and silane coupling agent application. This result is
consistent with data reported in previous studies.9,12 How-
ever, there is some evidence that suggests a significant

Vol 21, No 5, 2019 439

Emsermann et al

Table 4 Results of the failure mode analysis

Material Failure G1-NO G2-GB G3-GB- SI G4-HF-SI G5-SC-SI G6-MS G7-MS- SI G8-MS-MP
Brilliant adhesive 19 10 6 19 8 17 6 8
Crios
mixed (m1/m2)   8 (5/3) 13 (9/4)   10 (8/2) 3 (0/3) 12 (3/9) 10 (0/10)

cohesive (c1/c2)   2 (0/2)         2 (1/1) 2 (1/1)

Cerasmart adhesive 20 3 4 18 11     18

mixed (m1/m2)   14 (0/14) 16 (1/15)   7 (0/7)     2 (0/2)

cohesive (c1/c2)   3 (0/3)            

Lava adhesive 19 9 15 14 15 3 1  
Ultimate
mixed (m1/m2/m3)   11 (11/0/0) 3 (3/0/0) 3 (3/0/0) 3 (3/0/0) 17 (5/12/0) 17 (2/14/1) 20 (4/14/2)

cohesive (c1/c2)             1 (1/0)  

VITA adhesive 20 8 3 2        
Enamic
mixed (m1/m2/m3)   12 (11/1/0) 15 (15/0/0) 16 (16/0/0) 18 (18/0/0)     9 (4/2/3)

cohesive (c1/c2)               11 (10/1)

m1 = adhesive and within resin luting material, m2 = adhesive and within the substrate, m3 = adhesive and within resin luting material and substrate,
c1 = cohesive within the resin luting material, c2 = cohesive within the substrate.

beneficial effect of HF etching and silanization on bond
strength.23 Etchable filler particles are a prerequisite for the
efficacy of HF as a surface pretreatment for CAD-CAM com-
posite resins. Whereas fillers like zirconia are not etchable,
HF etching causes a superficial dissolution of etchable ce-
ramic filler components.38 However, HF etching may totally
dissolve some glass filler particles that are embedded in the
polymer matrix of indirect composite resins.31 The results of
the present study suggest that, in terms of the adhesive
performance, grit blasting is a more reliable surface pre-
treatment than HF etching for CAD-CAM composite resins.
HF etching of PICN materials has a more favorable effect
on the interfacial fracture toughness than grit blasting,10
and HF etching plus silane application, as recommended by
the manufacturer, is considered the preferred surface pre-
treatment for VITA Enamic.8,12,16,23 However, strong acid
etching protocols with 10% HF dissolve a great amount of
the glass phase, thus exposing the polymer structure; this
may minimize the efficacy of silane coupling agents owing
to the reduced silica content on the surface.21 Therefore,
the use of a mild etching protocol that roughens the sur-
face while preserving most of the silica content is recom-
mended to treat PICN materials.21
Silane application did not benefit the adhesive perfor-
mance of the resin luting material on CAD-CAM composite
resins in the present study. This is in line with data from
previous studies.7,31 Moreover, the results for Brilliant Crios
and Lava Ultimate demonstrate that the use of a universal
adhesive that acts as a resin primer has a favorable impact
on the adhesive performance. Recent studies have also
shown that an adhesive agent containing functional methyl-
methacrylates contributes more to the bonding between
CAD-CAM composite resin and resin luting material than a
silane primer.25,30,37 In fact, the use of a silane primer
without an adhesive coupling agent does not achieve high
bond strengths on CAD-CAM composite resins.30 This may
be due to the fact that inorganic filler particles are fre-
quently treated with silane coupling agents in the manufac-
turing process because incorporation of silanized filler par-
ticles in the resin matrix can increase the mechanical
strength and optimize the hydrolytic stability of composite
resins.20 In addition, the use of a silane coupling agent
alone is not adequate for bonding to non-silica–based filler
particles such as zirconia. Consequently, inorganic compo-
nents available as targets for silanization may be scarce
after mechanical roughening.30 Dispersed fillers that are
industrially treated with silane coupling agents are hydro-
phobic, and the nonhydrolyzable functional parts of the si-
lane coupling agents remain readily available for copolymer-
ization with methacrylate groups of the resin luting
material.20 The application of a silane primer can therefore
have no or even detrimental effects on the adhesive perfor-
mance of CAD-CAM composite resins. A further factor con-
tributing to the ineffectiveness of silanization may be incom-
plete evaporation of the solvent of the silane primer.11
Moreover, one should take into account that in the present
investigation, a single-phase silane primer was used, and
there is some evidence suggesting that two-component si-
lane primers, with their more controllable hydrolysis, might
be more effective than single-phase primers.11 Interestingly,
the use of the silane coupling agent from the same manu-
facturer as the PICN material significantly improved the ad-

440 The Journal of Adhesive Dentistry


hesive performance compared with a standard silane cou-
pling agent in the present study. The composition of these
silane primers, as labelled on the technical data sheets, is
identical apart from the solvent (Ultradent Silane, isopropyl
alcohol; Vitasil, ethanol). However, information on the 3-tri-
methoxysilylpropyl methacrylate loads is ambiguous. The
bond strength disparity is, therefore, most likely the result
of different 3-trimethoxysilylpropyl methacrylate loads.
Favorable bond strengths were obtained with both univer-
sal adhesives used in the present study. However, adhe-
sives differ in their efficiency as material primer.1,7,30,37
Universal adhesives that contain silane and phosphate
monomers in addition to regular methacrylate monomers
outperform adhesives based exclusively on methacrylic
monomers.37 Methacrylates contained in adhesive coupling
agents can, by radical polymerization, chemically bond to
unpolymerized methacryloyl groups in CAD-CAM composite
resins.30,43 Another adhesion mechanism is the interpene-
trating network formed when monomers of the universal
adhesives penetrate the resin matrix of CAD-CAM compos-
ite resins and polymerize there.25 Furthermore, silane cou-
pling agents or, more likely, phosphate monomers in univer-
sal adhesives enhance the bonding performance on
roughened CAD-CAM composite resins as they prime the
inorganic filler particles.37 The self-etching 10-methacryloy-
loxydecyl dihydrogen phosphate (10-MDP) monomer, con-
tained in the universal adhesives used in the present study,
is a primer for zirconia, alumina, metals, and dispersed zir-
conia fillers of composite resins.6 In addition, chemical
bonding to the organic phase may be achieved through acid
groups of the copolymers and 10-MDP contained in univer-
sal adhesives.26 Thus, universal adhesives may establish
adhesion to the organic phase as well as the filler particles
of CAD-CAM composite resins.25,43
Certain universal adhesives incorporate a silane cou-
pling agent, which should give the adhesive the potential
to directly bond to glass-rich ceramics. However, silanol is
unstable in the acidic solution of universal adhesives,
which promotes hydrolysis and dehydration condensa-
tion.42 Thus, silane coupling agents that are incorporated
in universal adhesives are insufficiently effective in chem-
ical bonding to glass-rich ceramics.42 It is currently un-
clear whether the bonding performance of universal adhe-
sives on CAD-CAM composite resins remains stable over
the long term.42 Therefore, the adequacy of universal ad-
hesives as supplementary material primers or substitutes
for silane coupling agents warrants further comparative
investigation.
The aim of this study was to assess the influence of a
variety of surface pretreatments on the adhesive perfor-
mance and not to compare bond strengths between differ-
ent materials. The results of the present study suggest that
it may be advantageous to use the luting materials that are
recommended by the manufacturer of the respective CAD-
CAM material. Significant interactions exist between differ-
ent resin luting materials and surface pretreatments. In ad-
dition, resin luting materials differ in their chemical
composition, physicomechanical properties, and wettabil-
Vol 21, No 5, 2019
Emsermann et al
ity.39 These differences may affect the bonding perfor-
mance on different CAD-CAM materials.23
Self-adhesive resin luting materials, ie, resin-based luting
agents that require no pretreatment of dental hard tissues
with either etch-and-rinse or self-etch adhesives, can offer
some advantages in clinical workflows owing to their more
straightforward application.19 However, limited information
is available concerning the efficacy of self-adhesive resin
luting materials on CAD-CAM composite resins.43 A small-
scale trial with a short follow-up of one year reported no
significant differences in the clinical performance of indirect
composite resin inlays and onlays bonded with either a self-
adhesive resin luting material or a conventional resin luting
material.19 Furthermore, in vitro studies demonstrate that
RelyX Unicem 2, a self-adhesive resin luting material, yields
favorable bond strengths to CAD-CAM composite resins as
well as VITA Enamic.29,43 In general, however, in vitro stud-
ies indicate that self-adhesive resin luting materials are in-
ferior to multistep resin luting materials for the bonding of
indirect composite resins.23,33 A systematic evaluation of
the adhesive performance of different resin luting materials
was beyond the scope of the present investigation, which
aimed, first and foremost, to assess the influence of differ-
ent surface pretreatment protocols. The resin luting mater-
ial had no significant impact on the adhesive performance
of the CAD-CAM composite resins. It is noteworthy, how-
ever, that conventional resin luting materials achieved
slightly higher – albeit not statistically significantly different
– bond strengths on these CAD-CAM materials. On the
whole, the results of the present study suggest that the
surface pretreatment protocol is more decisive than the
resin luting material and that, in terms of bond strength, the
use of conventional resin luting materials may offer some
advantages over self-adhesive resin luting materials.
Certain inherent limitations of the present in vitro study re-
quire careful consideration. First, the roughness that results
from milling varies with tool grit size, and this may in turn af-
fect micromechanical interlocking between CAD-CAM materials
and resin luting material and thus the strength of the adhesive
interface.15 In the present study, wet grinding of the samples
ensured a surface roughness comparable to that obtained by
CAD-CAM milling. However, no standard protocols for the sam-
ple preparation of CAD-CAM materials for bond strength test-
ing exist, which restricts comparability across studies.
Second, no standardized procedure for the artificial
aging of resin luting materials is available at present.3 The
effect of different surface pretreatments on bond strengths
was assessed after 6 months of water storage in the pres-
ent study. The storage time was chosen based on a previ-
ous study.7 When comparing bond strengths across differ-
ent studies, it is important to bear in mind that different
aging procedures and durations may have a strong impact
on the bonding performance.3
Third, in the present study, bond strength was assessed
with the Swiss shear test, a methodical approach that takes
polymerization shrinkage and stress into account.13 Micro-
tensile bond strength (μTBS) testing has a higher reliability
than (micro)shear bond strength testing.10,28 However,
441
Emsermann et al
μTBS testing may result in inaccuracies in bond strength
evaluation owing to an increased risk of pre-test failures dur-
ing specimen preparation and problems related to uneven
stress distribution.10,28 Shear bond strength tests are cur-
rently the most straightforward approach to obtain reliable
results,40 which is why this test method was chosen in the
present study. Nevertheless, the shortcomings inherent to
macroshear bond testing set-ups must not be overlooked.4
A high frequency of cohesive failures is a common occur-
rence with macro bond test methods and a proper assess-
ment of the interfacial bond strength is thus impossible.4
More reliable methods that offer insight into fracture me-
chanics and allow a quantitative assessment of interfacial
fracture toughness have been proposed for the evaluation
of adhesive interfaces.10,28,40 Moreover, elastic modulus
mismatches between bonded substrates have a determin-
ing influence on stress concentrations at the adhesive inter-
face when macro shear bond testing is performed.4 The
elastic moduli of the CAD-CAM materials tested in the pres-
ent study differ markedly.2,14 For example, the elastic modu-
lus of Cerasmart is lower than the one of Lava Ultimate,
which, in turn, has a lower elastic modulus compared with
VITA Enamic.2,14 The elastic constants of different resin lut-
ing materials, too, show considerable differences,27 which
may explain to some extent why some resin luting materials
obtained more favorable results on certain CAD-CAM mater-
ials than others in the present investigation.
CONCLUSION
Grit blasting had a more favorable effect on the adhesive
performance on CAD-CAM composite resins than HF etching
and tribochemical silica coating. In addition, the application
of a silane coupling agent may negatively affect the bond
strength on CAD-CAM composites whereas universal adhe-
sives show considerable potential as material primers. For
the PICN material VITA Enamic, surface pretreatment ac-
cording to the manufacturer’s recommendations combined
with the recommended products yielded the best bond
strengths.
ACKNOWLEDGMENTS
We thank Fredy Schmidli for his valuable technical assistance. Urs
Simmen, PhD, is gratefully acknowledged for his statistical consult-
ing service and contractual data analysis. Thanks are also due to
3M Oral Care, Coltène/Whaledent, GC Europe, and VITA Zahnfabrik
for generously providing the CAD-CAM materials and luting agents.
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43. Yu H, Yoshida K, Cheng H, Sawase T. Bonding of different self-adhesive
resins to high-strength composite resin block treated with surface condi-
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44. Zimmermann M, Koller C, Reymus M, Mehl A, Hickel R. Clinical evalu-
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Clinical relevance: Grit blasting and the application
of a suitable material primer is a useful surface pre-
treatment for reliable bonding of CAD-CAM composite
resins. For VITA Enamic, a PICN material, the bonding
protocol recommended by the manufacturer in combina-
tion with the recommended luting materials should be
followed to achieve a favorable adhesive performance.

Erratum

Erratum in:
J Adhes Dent 2019;21(4):355–363

Impact of Acid Concentration and Firing on the Long-term

Bond Strength of a Zirconia-Lithium Silicate Ceramic
Following Adhesive Cementation
Diniz, Vandeberg / Monteiro, Jaiane Bandoli / Rodrigues, Jonas Vinicius Meireles /
Prado, Pedro Henrique Condé Oliveira / Melo, Renata Marques de

On page 355, the date of submission is false.

Erratum for:
J Adhes Dent 2019;21(5):443.

The date of submission has been changed to 25.11.18.

Vol 21, No 5, 2019 443