Do Different Application Modes Improve the Bonding

Performance of Self-etching Ceramic Primer to Lithium

Disilicate and Feldspathic Ceramics?
Andres Felipe Millan Cardenasa / Angela Sisley Quintero-Calderonb / Fabiana Suelen Figuerêdo de
Siqueirac / Veridiana Silva Camposd / Michel Wendlingere / Camilo Andres Pulido-Moraf /
María José Masson-Palaciosg / Martha Lucia Sarmiento-Delgadoh / Alessandro D. Loguercioi

Purpose: To evaluate the effect of different application modes of a recently introduced self-etching ceramic primer
on the microshear bond strength (μSBS) and ceramic surface-etching pattern of two glass-ceramic surfaces.
Materials and Methods: Twenty-two CAD/CAM blocks of lithium disilicate (LD) and feldspathic glass ceramic (VTR)
were each cut into 4 rectangular sections (n = 88 for ceramic surface). The LD and VTR specimens were divided
into one control group (hydrofluoric acid + silane coupling agent [HF+SII]), and 10 experimental groups using Mono-
bond Etch and Prime (MEP) applied for a combination of scrubbing times (5, 10, 20, 40, and 60 s) and reaction
times (20 or 40 s). After each treatment, Tygon matrices (n = 8) were filled with a resin cement and light cured for
each ceramic specimen. The specimens were stored in water at 37°C for 24 h and subjected to the μSBS test. The
failure pattern and μSBS were statistically evaluated (α = 0.05). In addition, the ceramic surface etching pattern
was analyzed using scanning electron microscopy.
Results: For the LD groups, the application of MEP 60/40 resulted in a higher mean μSBS compared to HF+SI
(p < 0.05). Groups 5/40, 10/40, and 20/40 resulted in mean μSBS similar to that obtained by HF+SI (p > 0.05).
For VTR, no significant difference was observed among the groups (p = 0.32). Compared with MEP, HF better pro-
moted the dissolution of glass matrix for both ceramics. However, prolonged MEP scrubbing or reaction caused sig-
nificant dissolution of the glass matrix for both evaluated ceramics.
Conclusion: Active and prolonged application of MEP may be a viable alternative to HF+SI for increasing the bond
strength to LD.
Keywords: hydrofluoric acid, lithium disilicate, scanning electron microscopy, self-etching ceramic primer.

J Adhes Dent 2019; 21: 319–327. Submitted for publication: 23.08.18; accepted for publication: 14.04.19
doi: 10.3290/j.jad.a42929

M inimally invasive dentistry has been promoted and en-

abled by the use of indirect restorations constructed
with materials that have better mechanical properties.
Nowadays, different materials with esthetic properties and
clinical indications are used as indirect restorative materi-
als.16,21

a Professor, Postgraduate Program in Dentistry, CEUMA University, São Luis,
MA, Brazil. Research idea, designed testing assembly, performed bond
strength experiments, co-wrote paper.
b MSc Student, Department of Dentistry, National University of Colombia, Bo-
gota, Colombia. Performed microshearbond strength experiments, co-wrote
paper.
c Professor, Postgraduate Program in Dentistry, CEUMA University, São Luis,
MA, Brazil. Research idea, designed testing assembly, performed bond
strength experiments, co-wrote paper.
d PhD Student, Department of Restorative Dentistry, State University of Ponta
Grossa, Ponta Grossa, PR, Brazil. Research idea, designed testing assembly,
co-wrote paper.
e Undergraduate Student, Department of Dentistry, CEUMA University, São Luis,
MA, Brazil. Performed scanning electron microscopy, co-wrote paper.
f Professor, Department of Dentistry, National University of Colombia, Bogota,
Colombia. Designed testing assembly and contributed to the discussion.
g Professor, Department of Dentistry, Equinoccial Technological University,
Quito, Ecuador. Contributed substantially to discussion.
h Professor, Department of Dentistry, National University of Colombia, Bogota,
Colombia. Provided consulting for statistical analysis, co-wrote paper.
i Professor, Department of Restorative Dentistry, State University of Ponta
Grossa, Ponta Grossa, PR, Brazil. Provided consulting for statistical analysis,
contributed substantially to the discussion, proofread the manuscript.
Correspondence: Prof. Dr. Andres Felipe Millan Cardenas, Department of Post-
graduate Program in Dentistry, Universidade CEUMA, Rua José Montello 1,
Jardim Renascença, São Luís, Maranhão, Brazil. 65075120. Tel: +55-98-3214-
4164; e-mail: andresfelipemillancardenas@hotmail.com

Vol 21, No 4, 2019 319

Cardenas et al
Lithium disilicate
glass ceramic
(EMX, IPS e.max
CAD)
Monobond Etch &
Prime (MEP)
Feldspathic glass
ceramic
(VTR, Vitablocs
RealLife)
Fig 1 Flow chart of the experimental design.
Among these materials, polycrystalline ceramics are con-
sidered a “glass-free matrix” due to the absence of a glass
phase; they provide strength and fracture toughness but
with limited translucency.3,5 Due to the nature of polycrys-
talline ceramics, etching with hydrofluoric acid (HF) is diffi-
cult, and consequently, creating reliable, durable bonding is
challenging.33 For this reason, different surface treatments
have been suggested to increase the bond strength of resin
luting cements to polycrystalline ceramics.33
On the other hand, the esthetics and optical properties of
glass-matrix ceramics such as lithium disilicate and feldspathic
glass ceramics are superior to those of glass-free matrices.16
However, to achieve successful bonding during cementation of
glass-matrix ceramics, prior conditioning of the intaglio surface
with HF and a silane coupling agent (SI) is a standard proce-
dure for adhesive cementation,5 and are essential steps that
will influence the success of the restoration.9,44
Etching with HF can selectively dissolve the glass-matrix
ceramic and generate multiple roughness patterns on the
ceramic surface, which promotes microretention.8,18,22 After
HF, a silane is applied. Silane is a bifunctional molecule that
induces a chemical interaction between the silica in the
glass phase of the ceramic and the methacrylate groups of
the resin monomers through siloxane bonds,14,30,41 thereby
increasing the bonding strength.10,14,41 However, these ap-
plication steps increase the chairside time, and conse-
quently, the risk of mistakes during the bonding procedures.
To simplify this conditioning procedure, a self-etching ce-
ramic primer, Monobond Etch & Prime (MEP),19 which si-
multaneously etches and silanizes the intaglio surface of
320
Control group:
HF + Silane (HF + SI)
MEP 5/20
MEP 10/20
MEP 20/20 Microshear bond strength
(μSBS)
MEP 40/20
MEP 60/20
Ceramic surface etching
MEP 5/40 pattern
MEP 10/40
MEP 20/40
MEP 40/40
MEP 60/40
the glass-matrix ceramic restoration, was recently intro-
duced on the market. As per manufacturer’s recommenda-
tion, MEP should be scrubbed on the ceramic surface for
20 s and then left to react for 40 s. Regarding this proto-
col, several studies recently concluded that the bond
strength to lithium disilicate when using MEP was similar to
that achieved by the gold standard protocol (HF +
SI);1,13,35,39 however, the etching pattern produced by MEP
was inferior to that produced by HF.1,13,29,35,39 Neverthe-
less, to the best of our knowledge, different application pro-
tocols of this new self-etching ceramic primer have not yet
been evaluated, and it is known that different application
modes influence the bond strength to lithium disilicate.15,20
In addition, according to the manufacturer, MEP is used for
conditioning glass-matrix ceramic restorations; however, to
our best knowledge, only a few studies have evaluated the
conditioning of MEP on different ceramics.13,29,35,42
Thus, the aim of the present study was to evaluate the mi-
croshear bond strength (μSBS) and etching pattern of MEP
when applied using different application modes to two different
glass-matrix ceramics, and compare them with the perfor-
mance of HF + SI. The null hypotheses were as follows: the
different MEP application protocols have no influence on 1) the
microshear bond strength and 2) the etching pattern for the
two glass ceramics, as compared to those yielded by HF + SI.
The Journal of Adhesive Dentistry
 Cardenas et al

Table 1 Materials used, composition, application mode, and batch number

Material (manufacturer) Composition Application mode* Batch number

Condac porcelana 5%, (FGM Hydrofluoric acid, water, thickener, Apply for 20 s, rinse with water for 30 s, 110615
Prod Odonto; Joinville, SC, surfactant, coloring clean ultrasonically with distilled water
Brazil) for 180 s

Vita Ceramics 5% Etch (Vita Sulfuric acid, hydrofluoric acid, ethanol Apply for 60 s, rinse with water for 30 s, 42530
Zahnfabrik; Bad Säckingen, clean ultrasonically with distilled water
Germany) for 180 s

Monobond Plus (Ivoclar Ethanol, 3-trimethoxysilylpropyl Apply with a brush and allow to react for 1401001210
Vivadent; Schaan, methacrylate, methacrylated phosphoric 60 s, disperse excess with a strong
Liechtenstein) acid ester (10-MDP), disulfide acrylate stream of air to ensure solvent
evaporation*

Monobond Etch & Prime (Ivoclar Butanol, tetrabutylammonium Apply onto the luting surface with a U10661
Vivadent) dihydrogen trifluoride, methacrylated microbrush and rub for 20 s, leave on
phosphoric acid ester, trimethoxypropyl on the surface for a further 40 s, rinse
methacrylate monomer thoroughly, dry for 10 s

Variolink II (Ivoclar Vivadent) Urethane dimethacrylate, inorganic Mix at a 1:1 ratio on a mixing pad, pack U50748
fillers, ytterbium trifluoride, initiators, resin cement carefully inside each tube,
stabilizers, pigments light cure for 20 s at 1200 mW/cm2

*According to manufacturers’ recommendations.

MATERIAL AND METHODS
Specimen Preparation
Two CAD/CAM materials were selected: 1) lithium disilicate
(EMX, IPS e.max CAD, Ivoclar Vivadent; Schaan, Liechten-
stein) and 2) feldspathic glass ceramic (VTR, Vitablocs Re-
alLife, VITA Zahnfabrik; Bad Säckingen, Germany).
Twenty-two CAD/CAM blocks of each material were used.
For each material, the blocks (12 x 12 x 6 mm) were cut
into 4 rectangular sections (6 x 6 x 6 mm) (n = 88 per ce-
ramic surface) using a diamond disk at slow speed (Isomet,
Buehler; Lake Bluff, IL, USA) under water cooling. After
cleaning ultrasonically with distilled water for 15 min, the
EMX specimens were fired in a furnace (Programat P300,
Ivoclar Vivadent) following the crystallization program at
840–850ºC for 20–31 min.
Experimental Design
For each indirect material, the specimens were randomly
assigned (http://www.sealedenvelope.com) into 11 groups
(n = 8), with 66 specimens used for the μSBS test and 22
specimens used to evaluate the ceramic surface-etching
pattern according to the following independent variables. In
the control group (HF+SI) 5% HF (FGM; Joinville, SC, Brazil)
+ silane coupling agent (Monobond P, Ivoclar Vivadent)
were applied according to the manufacturer’s recommenda-
tions for each ceramic surface. For EMX, HF 5% was applied
for 20 s, followed by rinsing with water for 30 s, ultrasonic
cleaning in water for 180 s and silane application for 60 s.
For VTR, HF 5% was applied for 60 s, followed by rinsing
with water for 30 s, ultrasonic cleaning in water for 180 s,
and silane application for 60 s, and Monobond Etch and
Prime (MEP; Ivoclar Vivadent) was applied with scrubbing
for 5, 10, 20, 40, and 60 s and left to react for 20 or 40 s
(Fig 1). The composition, application mode, batch number,
and experimental groups are described in Tables 1 and 2.
Microshear Bond Strength Test
The specimens (n = 66) were mounted on a polyvinyl chloride
(PVC) ring filled with acrylic resin (AutoClear, DentBras; Piras-
sununga, SP, Brazil), where the specimen surface was ex-
posed on the top of the cylinder with a height of 3 mm.
The specimens were etched according to the different
experimental protocols (Fig 1) and thoroughly rinsed with
water spray. Monobond P or MEP (Ivoclar Vivadent) was ap-
plied according to the respective manufacturer’s instruc-
tions and experimental groups (Table 1). A single operator
performed all the bonding procedures. Then, eight transpar-
ent polyethylene Tygon tubes (Tygon Medical Tubing Formu-
lations 54-HL, Saint Gobain Performance Plastics; Akron,
OH, USA) with an internal diameter of 0.8 mm and a height
of 0.5 mm were positioned over each ceramic specimen.
The resin cement Variolink II (Ivoclar Vivadent) (Table 1)
was carefully packed inside each tube, and a clear Mylar
matrix strip was placed over the filled Tygon tube and
pressed gently into place. The luting composite specimens
were simultaneously light cured for 20 s using an LED light-
curing unit set at 1200 mW/cm2 (Radii-cal, SDI; Bayswater,
Victoria, Australia) in close contact with the Mylar strip. A
radiometer (Demetron LED Radiometer, Kerr Sybron Dental

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Table 2 Surface ceramic and application mode of experimental groups

Ceramic Etching Experimental Application mode Resin

surface agent groups cement
Lithium Hydrofluoric 1. Control group: 1. 5% hydrofluoric acid etching for 20 s Variolink II*
disilicate acid (HF) HF + silane (HF + 2. Rinse with water for 30 s
glass ceramic SI) 3. Clean ultrasonically with distilled water for 180 s
(EMX, IPS 4. Apply silane solution and Monobond Plus* with a brush and allow to react for 60 s.
e.max CAD)* Subsequently, disperse the excess with a strong stream of air to ensure solvent
evaporation*

Monobond 1. MEP scrubbing for 5 s, let react on the surface for 20 s Rinse thoroughly, dry Variolink II*
Etch & Prime 2. Group 5/20 2. MEP scrubbing for 10 s, let react on the surface for 20 s for 10 s
(MEP) 3. Group 10/20 3. MEP scrubbing for 20 s, let react on the surface for 20 s
4. Group 20/20 4. MEP scrubbing for 40 s, let react on the surface for 20 s
5. Group 40/20 5. MEP scrubbing for 60 s, let react on the surface for 20 s
6. Group 60/20 6. MEP scrubbing for 5 s, let react on the surface for 40 s
7. Group 5/40 7. MEP scrubbing for 10 s, let react on the surface for 40 s
8. Group 10/40 8. MEP scrubbing for 20 s, let react on the surface for 40 s*
9. Group 20/40 9. MEP scrubbing for 40 s, let react on the surface for 40 s
10. Group 40/40 10. MEP scrubbing for 60 s and left to reacted on the
11. Group 60/40 surface for 40 s

Feldspathic Hydrofluoric 1.Control group: 1. 5% hydrofluoric acid etching for 60 s VariolinkII*

glass ceramic acid (HF) HF + Silane (HF + 2. Rinse with water for 30 s
(VTR, SI) 3. Clean ultrasonically with distilled water for 180 s
Vitablocs 4. Apply silane solution and Monobond Plus* with a brush and allow to react for 60 s.
RealLife)** Subsequently, disperse the excess with a strong stream of air to ensure solvent
evaporation*

Monobond 1. MEP scrubbing for 5 s, let react on the surface for 20 s Rinse thoroughly, Variolink® II*
Etch & Prime 2. Group 5/20 2. MEP scrubbing for 10 s, let react on the surface for 20 s dry for 10 s
(MEP)*** 3. Group 10/20 3. MEP scrubbing for 20 s, let react on the surface for 20 s
4. Group 20/20 4. MEP scrubbing for 40 s, let react on the surface for 20 s
5. Group 40/20 5. MEP scrubbing for 60 s, let react on the surface for 20 s
6. Group 60/20 6. MEP scrubbing for 5 s, let react on the surface for 40 s
7. Group 5/40 7. MEP scrubbing for 10 s, let react on the surface for 40 s
8. Group 10/40 8. MEP scrubbing for 20 s, let react on the surface for 40 s*
9. Group 20/40 9. MEP scrubbing for 40 s, let react on the surface for 40 s
10. Group 40/40 10. MEP scrubbing for 60 s and left to reacted on the
11. Group 60/40 surface for 40 s

* According to the manufacturer’s (Ivoclar Vivadent) recommendations; ** Vita Zahnfabrik; *** the manufacturer of MEP did not have a specific application
protocol for Vita Blocs.

Specialties; Middleton, WI, USA) was used to check the
light intensity every 8 specimens. These procedures were
carried out under magnifying loupes.27
After storing the specimens in distilled water for 24 h at
37°C, the Tygon tubes were carefully removed with a blade,
exposing the cement cylinders. Each specimen was exam-
ined under a stereomicroscope at 10X magnification. The
cement cylinder was discarded if pores or gaps were ob-
served at the interface. The specimens were attached to a
shear-testing fixture (Odeme Biotechnology; Joaçaba, SC,
Brazil) and tested in a universal testing machine (Kratos
IKCL 3-USB, Kratos Equipamentos Industriais; Cotia, SP,
Brazil). Each specimen was positioned in the universal test-
ing machine and a thin orthodontic wire (0.2 mm diameter)
was looped around the base of each composite cylinder.
The orthodontic wire contacted the composite cement cylin-
der on half of its circumference. The setup was kept aligned
(cement-ceramic interface, the wire loop, and the center of
the load cell) to ensure correct orientation of the shear
forces.37 The crosshead speed was set at 1 mm/min until
failure.
The μSBS (in MPa) was calculated by dividing the load at
failure by the surface area (mm2) of each specimen. After
testing, the specimens were examined under an optical mi-
croscope (SZH-131, Olympus; Tokyo, Japan) at 100X mag-
nification to identify the location of bond failure. The failure
mode was classified as cohesive in resin cement (CR), that
is, failure exclusively within the resin cement; cohesive in
ceramic (CC), ie, failure exclusively within the ceramic; ad-
hesive (A), ie, failure at the resin cement-ceramic interface;
and mixed (M), that is, failure included cohesive failure of
the neighboring substrates.
Ceramic Surface-etching Pattern
To etch surfaces, the specimens (n = 22) of each ceramic
were surface conditioned with HF or MEP according to the
experimental conditions previously described (Table 1).
Then, the specimens were rinsed and dried. Furthermore,
two additional surfaces of each ceramic (6 x 6 x 6 mm) were
added to evaluate the non-conditioned ceramic surface. All
the specimens were dried and dehydrated in a desiccator
for 12 h, and the conditioned ceramic surfaces were sputter

322 The Journal of Adhesive Dentistry

 Cardenas et al

Table 3 Number of specimens (%) according to fracture mode for all experimental groups

EMX VTR

Experimental groups A M CR CC A M CR CC
Hydrofluoric acid + silane 43 (90) 5 (10) 0 (0) 0 (0) 31 (68) 7 (15) 2 (4) 6 (13)
MEP 5/20 45 (94) 1 (2) 2 (4) 0 (0) 40 (84) 2 (4) 0 (0) 6 (12)
10/20 46 (98) 1 (2) 0 (0) 0 (0) 43 (90) 2 (4) 0 (0) 3 (6)
20/20 45 (94) 3 (6) 0 (0) 0 (0) 44 (94) 1 (2) 0 (0) 2 (4)
40/20 41 (85) 7 (5) 0 (0) 0 (0) 29 (60) 3 (7) 2 (4) 14 (29)
60/20 41 (85) 6 (11) 2 (4) 0 (0) 31 (65) 5 (10) 0 (0) 12 (25)
5/40 48 (100) 0 (0) 0 (0) 0 (0) 41 (84) 3 (6) 2 (4) 3 (6)
10/40 48 (100) 0 (0) 0 (0) 0 (0) 39 (81) 2 (2) 1 (2) 6 (13)
20/40 40 (84) 5 (10) 3 (6) 0 (0) 28 (59) 6 (13) 6 (13) 7 (15)
40/40 44 (92) 4 (8) 0 (0) 0 (0) 34 (71) 6 (12) 0 (0) 8 (17)
60/40 41 (85) 7 (15) 0 (0) 0 (0) 27 (57) 7 (15) 1 (2) 12 (26)
EMX: lithium disilicate; VTR: feldspathic glass ceramic. Fracture modes: A: adhesive; m: mixed; CR: cohesive in resin cement; CC: cohesive in ceramic.

Table 4 Mean (± SD) microshear bond strengths in MPa for all experimental groups

Experimental groups EMX VTR

Hydrofluoric acid + silane 31.17 ± 1.0 B 27.62 ± 1.5 a
MEP 5/20 14.43 ± 0.3 D 27.61 ± 1.3 a
(scrubbing time/reaction time)
10/20 20.00 ± 1.5 C 27.31 ± 2.5 a
20/20 25.07 ± 0.8 C 28.15 ± 1.9 a
40/20 32.40 ± 1.8 AB 27.70 ± 1.6 a
60/20 33.57 ± 1.1 AB 29.10 ± 1.2 a
5/40 32.03 ± 1.1 B 27.90 ± 1.0 a
10/40 31.50 ± 0.6 B 27.09 ± 1.4 a
20/40 33.27 ± 1.2 AB 27.78 ± 1.4 a
40/40 31.90 ± 1.7 AB 28.05 ± 1.3 a
60/40 35.30 ± 1.6 A 28.49 ± 0.3 a
Different capital (EMX) or lowercase letters (VTR) in each column indicate statistically significant differences for each material (one-way ANOVA, Tukey’s test,
p < 0.05)

coated with gold-palladium in a vacuum evaporator (SCD
050, Balzers; Schaan, Liechtenstein). The entire treated sur-
face was examined under a scanning electron microscope
(SEM, MIRA3 LM, Tescan Orsay Holding; Warrendale, PA,
USA), and three photomicrographs of representative surface
areas were taken at different magnifications.
Statistical Analysis
The data were first analyzed using the Kolmogorov-Smirnov
test to assess whether the data followed a normal distribu-
tion, after which Barlett’s test for equality of variances was
performed to determine if the assumption of equal vari-
ances was valid.26 After confirming the normality of data
distribution and the equality of the variances, the μSBS (in
MPa) data were subjected to appropriate statistical analy-
sis. The mean μSBS of all the specimens from the same
ceramic surface were averaged for statistical purposes.
One-way ANOVA was used to analyze the μSBS data for
each glass ceramic material. Tukey’s post-hoc test was ap-
plied with α = 0.05.

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Cardenas et al

a b c d e f

g h i j k l

Fig 2 Representative SEM images of EMX surface (25,000X): the untreated EMX surface does not show vitreous matrix dissoution (a).
EMX etched with 5% hydrofluoric acid for 20 s shows significant vitreous matrix dissolution and exposed crystals (arrow). Different etching
patterns observed for different MEP application modes (g). Poor vitreous matrix dissolution and exposed crystals can be observed in (b)
MEP-5/20, (c) MEP-10/20, (d) MEP-20/20, (h) MEP-5/40, and (i) 10/40. The increase in MEP application time leads to slightly greater
vitreous matrix dissolution with an increase in surface roughness, porosity (white hands), and exposed crystals (e, f, k, and l) when compared
to the manufacturer’s protocol (j).

RESULTS characterized by an increase in porosity and roughness and

Microshear Bond Strength
For each ceramic surface, the majority of specimens showed
adhesive failures, as shown in Table 3. For the lithium disili-
cate ceramic, there are significant differences among the
groups (ANOVA test; p = 0.001; Table 4). The application of
MEP 60/40 resulted in a higher mean μSBS than did the
application of HF + SI (Tukey’s test; p < 0.05; Table 4). The
mean μSBS of groups 5/40, 10/40, and 20/40 were simi-
lar to that of the HF + SI control group (Tukey’s test; p >
0.05; Table 4). On the other hand, groups 5/20, 10/20,
and 20/20 showed lower mean μSBS than that obtained by
the HF + SI control group (Tukey’s test; p < 0.05; Table 4).
For the feldspathic ceramic, there were no significant dif-
ferences among the groups (ANOVA; p = 0.32; Table 4).
That is, no significant differences were observed in the
mean μSBS when MEP was applied regardless of protocol,
as compared to the HF + SI control group (ANOVA; p = 0.32;
Table 4).
Ceramic Surface-etching Pattern
The representative SEM images of the ceramic surface-
etching patterns for different experimental groups are
shown in Figs 2 and 3. The untreated lithium disilicate and
feldspathic ceramics showed a smooth surface without any
craters or pits. HF promoted the dissolution of glass matrix,
exposure of vitreous matrix dissolution for both ceramics.
MEP caused partial dissolution of the vitreous matrix,
showing fewer pores and less pronounced roughness
(Figs 2 and 3). However, a progressive effect of the differ-
ent MEP application protocols was manifest as a greater
dissolution of the glass matrix of the ceramics with the for-
mation of larger, deeper craters and pits with increasing
scrubbing and reaction times (Figs 2 and 3), up to a total
application time of 60 s.
DISCUSSION
The results of the present study showed that the conven-
tional application of 5% HF followed by silane coupling
agent achieved a well-defined conditioning pattern and a
high μSBS to both of the evaluated glass-matrix ceramics.
This could be attributed to two factors: 1. the application of
HF resulted in some major pores with severe irregularities
on the intaglio ceramic surface,8,18,22 as observed in the
present study (Figs 2 and 3); 2. the use of a silane coupling
agent created a chemical bond between the ceramic and
the resin monomers,14,30,41 which increased the wettability
of the resin cement.5
However, due to the toxicity and volatility of HF, its use
has been questioned, especially given the potential health

324 The Journal of Adhesive Dentistry

 Cardenas et al

a b c d e f

g h i j k l

Fig 3 Representative SEM images of VTR surface (3000X): untreated VTR shows no pores or surface roughness (a). Dissolution of the
vitreous matrix with an aggressive etched pattern and deeper pores (white hands) can be observed on the VTR surface after etching
with hydrofluoric acid for 60 s (g). Progressive vitreous matrix dissolution can be observed for different MEP application protocols (b, c, d, h,
and i). A more aggressively etched pattern with major pores (white hands) and matrix dissolution can be observed with increasing MEP
application time (e, f, j, k, and l).

hazard upon contacting unprotected skin.4,32 This is a seri-
ous problem in intraoral ceramic repair.31 One alternative
evaluated in the present study is provided by the new self-
etching ceramic primer. According to the manufacturer, MEP
is less toxic and poses less health risk.19
Unfortunately, although MEP caused a partial dissolution
of the glass-ceramic matrix,19 it yielded a less-pronounced
etching pattern when to both the ceramic surfaces com-
pared to HF (Figs 2 and 3). This could be attributed to the
milder acidic nature of MEP, which has been previously re-
ported1,13,29,35,39 and could be responsible for the lower
bond strength (groups 5/20, 10/20, and 20/20) to lithium
disilicate ceramic at shorter application times.
However, the results of the present study showed that
active, prolonged application of MEP might compensate for
the milder etching potential of ammonium polyfluoride pres-
ent in MEP, which leads to the formation of several irregu-
larities and pores due to the dissolution of the glass matrix
(Figs 2 and 3). Moreover, although a longer scrubbing time
along with a longer reaction time of MEP did not yield the
same conditioning pattern as that of HF, but bond strengths
similar to that of HF + SI were obtained when the MEP ap-
plication time was at least 60 s (scrubbing + reaction time)
on the lithium disilicate ceramic surface.
The exact action mechanism of MEP is not entirely
clear.13,35,42 According to the manufacturer, MEP contains
functional monomers such as methacrylate phosphoric acid
ester (10-MDP), which is responsible for increasing the po-
tential for chemical interaction.11,19 In addition, MEP con-
tains trimethoxypropyl methacrylate (methacrylate silane),
which leaves a thin, chemically bonded layer of silane on
the surface even after washing with water and drying.19 It is
worth mentioning that silane coupling agents play an impor-
tant role in promoting bifunctional adhesion on a ceramic
surface.24,25 The presence of both molecules could be re-
sponsible for the lower contact angle with the glass ceramic
surface when MEP was applied.35,42
Further, it is noteworthy that some questions have been
raised regarding the stability of silane molecules in acidic
environments.20,48 Continuous hydrolyzation of silanol
groups occurs during long-term storage in a low-pH solution.
Therefore, although the manufacturer of MEP claims that
the silane coupling agent is stable during storage in the
presence of ammonium polyfluoride, this hypothesis needs
to be evaluated in the near future, since the condensation
reaction of the silanol groups is suppressed and the forma-
tion of a highly reactive monomeric silanol is continually
promoted at a steady rate during storage.19 Based on these
considerations, the bonding mechanism of MEP is expected
to be related to the interaction between the functional phos-
phoric monomers and ceramic ions rather than the methac-
rylate silane bonding to the glass ceramic.
Therefore, when MEP was applied for 60 s (reaction
time) instead of 20 s, the interaction of the acidic resinous

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monomers (methacrylated phosphoric acid ester) with the
ceramic surface improved, similar to that on enamel,
thereby increasing not only the potential of etching, but also
monomer impregnation into the underlying surface.34,43
Furthermore, 60 s of scrubbing application can not only
eliminate water, alcohol, and other products of the silane
reaction, but also help complete the condensation reaction
between silane and silica, promoting the formation of silox-
ane.36 Thus, evaporation of alcohol can increase the den-
sity of local connections available for the solution of silane
to react with the ceramic.36 Therefore, we hypothesized
that the prolonged, active application increased the poten-
tial of etching associated with solvent evaporation and
helped promote the formation of siloxane groups, thus im-
proving the μSBS for the lithium disilicate ceramic surface.
Figure 2 clearly shows the positive effect of active and
prolonged MEP application on the surface topography. How-
ever, the μSBS to the lithium disilicate surface did not show
an increasing trend, mainly after at least 20 s of scrubbing
(minimum 40 s of reaction; 20/40 and 40/40) or at least
40 s of scrubbing associated with a minimum 20 s of reac-
tion (40/20 and 60/20). It is known that the higher surface
roughness is not directly related to increased bond
strength.47,49 However, the presence of methacrylate phos-
phoric acid ester and methacrylate silane could be respon-
sible for the higher potential for chemical interaction11,19
and lower contact angle with the glass ceramic surface,35,42
which would make the surface changes less necessary.
This can also explain the absence of significant differ-
ences in the μSBS with even a slight increase in the etching
pattern upon MEP application to the feldspathic ceramic.
The results are in agreement with those of Venturi et al,46
who reported that increasing the etching pattern using a
higher concentration of HF did not result in any difference in
the bond strength for a feldspathic ceramic. It is known that
feldspathic ceramics have a higher amount of amorphous
glass matrix,17,38 and due to the micromechanical nature of
the adhesion between the ceramic surface and resin ce-
ment, any microtopographical change plays an important
role in its chemical adhesion with silane. Thus, we hypoth-
esized that irrespective of the active and prolonged applica-
tion, the microtopographical alterations on the feldspathic
ceramic surface created by MEP were sufficient to produce
bond strength simliar to that induced by HF + SI.
Additionally, the results revealed a strong association
between the failure mode, surface treatment, and type of
material. The highest percentage of adhesive failure was
observed for shorter application times (groups 5/20,
10/20, 20/20, 5/40, and 10/40) for the lithium disilicate
ceramic surface, while a high percentage of cohesive failure
was observed in feldsphatic glass ceramics independent of
surface treatment. These findings could be attributed to the
difference in the microstructure and the lower intrinsic
strength (brittleness) of the feldspathic ceramic. The addi-
tion of long lithium disilicate crystals results in greater flex-
ural strength and fracture resistance than feldspathic ce-
ramic, due to the spatial configuration of their crystalline
grid and resistance to crack propagation through crystals.2
326
It is worth mentioning that the occurrence of cohesive
failure could not be attributed to the load application de-
vice. Orthodontic wire was used in this study instead of a
chisel, because the former distributes stress more evenly
around the adhesive interface area6,12,45 as it has a large
contact area compared to a chisel.6,28 In contrast, a chisel
promotes puncture loading, resulting in a smaller contact
area and causing severe stress concentration at the load
application area, thus inducing a larger number of cohesive
failures.6,28 This is the reason that several recently pub-
lished papers used orthodontic wire instead of a chisel for
evaluating the μSBS of adhesive interfaces.7,22,23,28,35,40
Thus, the results of the present study lead to partial re-
jection of the first null hypothesis and complete rejection of
the second null hypothesis. However, further studies are
required to clarify the effect of different MEP application
protocols on the pretreatment of other glass-matrix ceram-
ics, mainly focusing on the chemical interaction with the
surface. Finally, although MEP showed good results in the
present study as in previous studies, future randomized
clinical studies are required to evaluate MEP as a condi-
tioner of glass ceramics.
CONCLUSION
Although the active and prolonged application of MEP re-
sulted in progressive glass matrix dissolution for both the
evaluated glass-matrix ceramics, none of the cases showed
an etching pattern similar to that obtained with traditional
HF treatment. MEP provided results similar to those ob-
tained with HF+SI, and active, prolonged application of MEP
improved the bond strength for lithium disilicate compared
to HF+SI. The scrubbing and application times of MEP were
material dependent.
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Clinical relevance: MEP provided results similar to
those of HF+SI. Active, prolonged application of MEP
may be a viable alternative for increasing the bond
strength only for lithium disilicate.
327