Efficacy of Various Surface Treatments on the Bonding

Performance of Saliva-contaminated Lithium-Disilicate

Ceramics
Sai Kham Lyanna / Tomohiro Takagakib / Toru Nikaidoc / Takahiro Wadad / Motohiro Uoe /
Masaomi Ikedaf / Alireza Sadrg / Junji Tagamih

Purpose: To investigate the efficacy of different ceramic surface cleaning methods after saliva contamination on
the resin bond strength to lithium disilicate ceramics.
Materials and Methods: 300 e.max CAD blocks (Ivoclar Vivadent) were polished with 600-grit silicon carbide paper
and divided into five groups with or without human saliva contamination and according to the surface treatment
performed (n = 10); control: no pretreatment; MP: Monobond Plus; PA+MP: 37% phosphoric acid (PA) followed by
MP; HF+MP: 5% hydrofluoric acid (HF) followed by MP; MEP: Monobond Etch & Prime. The specimens were bonded
with one of three resin cements: Variolink Esthetic DC (VE), Multilink Automix (MA) and Speed CEM (SC). After 24-h
water storage, tensile bond strength (TBS) was measured. The ceramic surfaces after pretreatment were analyzed
using x-ray photoelectron spectroscopy (XPS).
Results: XPS analysis showed similar elemental distributions between saliva contamination vs no saliva in PA, HF,
and MEP. The TBSs were significantly influenced by surface treatments (p < 0.05). HF+MP and MEP showed statisti-
cally non-significantly different bond strengths to saliva-contaminated HF+MP and MEP, but were different from MP
and saliva-contaminated MP. The TBSs after 24 h were significantly higher in HF+MP and MEP groups with VE. HF+MP
and MEP did not show statistically significant differences among any groups with or without saliva contamination.
Conclusion: Surface treatments with PA or HF followed by silane or by MEP alone were effective in removing saliva
contamination and enhancing the resin bond strength.
Keywords: lithium disilicate ceramics, saliva-contaminated, tensile bond strength.

J Adhes Dent 2019; 21: 51–58. Submitted for publication: 01.06.18; accepted for publication: 25.11.18
doi: 10.3290/j.jad.a41918

T he demands for esthetic restorations have increased

substantially in recent years, and the popularity of all-
ceramic materials as an alternative to metal-ceramic for in-
direct restorations has therefore grown. A weak point for all
ceramics is considered to be the extension and growth of
microscopic surface flaws, but the resistance to crack prop-
agation of ceramics has been improved by leucite, fluor-
mica, or alumina reinforcement of the glass matrix.23 Many
studies have documented the success of glass-ceramic
restorations bonded with resin-based cements. However, to

a Student, Cariology and Operative Dentistry, Graduate School of Medical and
Dental Sciences, Tokyo Medical and Dental University, Tokyo, Japan. Participated
in experimental design, performed the experiments, wrote the manuscript.
b Assistant Professor, Cariology and Operative Dentistry, Graduate School of Med-
ical and Dental Sciences, Tokyo Medical and Dental University, Tokyo, Japan.
Idea, hypothesis, experimental design, proofread the manuscript.
c Lecturer, Department of Operative Dentistry, Division of Oral Functional Sci-
ence and Rehabilitation, School of Dentistry, Asahi University, Gifu, Japan.
d ported the experiments, contributed substantially to discussion.
Assistant Professor, Advanced Biomaterials, Graduate School, Tokyo Medical
and Dental University, Tokyo, Japan. Contributed substantially to discussion,
proofread the manuscript.
e Professor, Advanced Biomaterials, Graduate School, Tokyo Medical and Dental
University, Tokyo, Japan. Contributed substantially to discussion, proofread the
manuscript.
f Junior Assistant Professor, Oral Prosthetic Engineering, Graduate School,
Tokyo, Japan. Performed a statistical analysis, contributed substantially to dis-
cussion.
g Associate Professor, Department of Restorative Dentistry, University of Wash-
ington School of Dentistry, Seattle, WA, USA. Contributed substantially to dis-
cussion, proofread the manuscript.
h Professor, Cariology and Operative Dentistry, Graduate School of Medical and
Dental Sciences, Tokyo Medical and Dental University, Tokyo, Japan. Sup-
Correspondence: Tomohiro Takagaki, Cariology and Operative Dentistry, Gradu-
ate School of Medical and Dental Sciences, Tokyo Medical and Dental University,
1-5-45, Yushima, Bunkyo-ku, Tokyo 113-8510, Japan. Tel: +813-5803-5483;
e-mail address: takagaki.ope@tmd.ac.jp

Vol 21, No 1, 2019 51

Lyann et al
Ultrasonic cleaning
(deionized water 5 min, immersed in human saliva (1 min.)
ethanol 2 min) and washed with water and air dried
air drying
IPS e.max CAD (5 mm x 15 mm)
•sintering
•polishing with #600 SiC paper
metal rod
The specimens were
resin cement
stored in deionized water
aluminium tape at 37°C for 24 h
e.max CAD block
Filled with resin cement
and light cured for 40 s
Fig 1 Schematic representation of specimen preparation design.
optimally create a resin-ceramic bond, glass-ceramic resto-
rations should be pretreated with hydrofluoric acid (HF) and
a silane coupling agent.22 HF creates porosities in the
glass ceramic, and the coupling agent serves the dual pur-
pose of binding to the silica of the ceramic and to the meth-
acrylate group of the adhesive resin.4,22
Ceramic etching with HF can be performed either at
chairside by the dentist or in the dental laboratory by the
dental technician. As a series of surveys on clinically used
adhesive ceramic bonding methods in Northern Germany
showed, there is still a considerable lack of understanding
about the principles of reliable ceramic bonding among den-
tal practitioners.15 When performed by the dental techni-
cian, the subsequent try-in procedure leads to surface con-
tamination with saliva.22 Saliva contains organic materials
such as salivary proteins, enzymatic molecules, bacteria
and food debris, and inorganic compounds such as mineral
ions in water.18 Adsorption of salivary proteins to dental
materials and tooth surfaces results in a pellicle consisting
of free (ie, planktonic) bacteria which develops to a thick-
ness of 10-20 nm within a few minutes.9 The resulting per-
sistent protein contamination from saliva in particular was
shown to hinder adhesion of the resin cements to ceram-
ics.7,21 Therefore, several cleaning methods have been pro-
posed to eliminate such contamination from the ceramic
52
Surface treatment
1. Control (no treatment)
2. No treatment + Monobond Plus (60 s)
3. Phosphoric acid (20 s) + Monobond Plus (60 s)
4. Hydrofluoric acid (20 s) + Monobond Plus (60 s)
5. Monobond Etch & Prime (scrub for 20 s, leave to
react for 40 s)
Failure mode
Tensile bond
strength test analysis by SEM
surface.1,16,29 In fact, due to the hazardous potential of HF,
its chairside application should be performed with cau-
tion.24 As a result, alternative cleaning methods without the
use of HF have been sought, including rinsing with water,25
etching with phosphoric acid, and cleaning with alcohol.34
Despite the fact that these methods are easy to apply, they
did not seem to recover the bonding capacity of ceramic
restorations compared to non-contaminated surfaces.25,34
Ammonium fluorides, especially ammonium bifluoride in
combination with other acids, have been investigated as a
possible etching media for dental ceramics for many
years.3,12,20 Recently, a single bottle ceramic self-etching
silane primer Monobond Etch & Prime (MEP, Ivoclar Viva-
dent; Schaan, Liechtenstein) was introduced. It has been
claimed that effects of MEP are comparable to those of HF
and silane treatment.19,26,30,33 However, details regarding
bonding efficacy, surface analysis, and detailed comparison
with existing cleaning materials after human saliva contam-
ination remain unclear.
Therefore, the purpose of this study was to investigate the
efficacy of different ceramic surface cleaning methods after
saliva contamination on the resin bond strength to lithium
disilicate ceramics. The null hypothesis was that the resin-
ceramic bond strength of the resin cements to the ceramics
was not influenced by contamination and cleaning method.
The Journal of Adhesive Dentistry
 Lyann et al

Table 1 Composition of the materials used in this study

Material Product Composition Batch No.

IPS e.max CAD Ivoclar Vivadent SiO2, Li2O, K2O, Al2O3, P2O5, ZrO2, ZnO, MgO, color oxides U37584

IPS Ceramic Etching Gel Ivoclar Vivadent < 5 % hydrofluoric acid T35311

Total Etch Ivoclar Vivadent Phosphoric acid (37 wt% in water), thickening agent and pigments V20970

Monobond Etch & Prime Ivoclar Vivadent Butanol, trimethoxypropyl methacrylate, tetrabutylammoniun dihydrogen
U20251
trifluoride, methacrylated phosphoric acid ester, colorant

Monobond Plus Ivoclar Vivadent Silane methacrylate, phosphoric acid methacrylate, ethanol and sulfide
T29123
methacrylate

Alloy primer Kuraray Noritake Dental Monomer MDP, triazine-based vinyl monomer, solvent (acetone) C80060

Urethane dimethacrylate and methacrylate monomers

Variolink Esthetic DC Ivoclar Vivadent Ytterbium trifluoride and spheroid mixed oxide V28271

Initiators, stabilizers and pigments

Mixed oxide

Multilink Automix Ivoclar Vivadent Dimethacrylate and HEMA U54978

Barium glass, ytterbium trifluoride and spheroid mixed oxide

Dimethacrylates and acidic monomers

Barium glass, ytterbium trifluoride, co-polymer and highly dispersed

SpeedCEM Ivoclar Vivadent V10538
silicon dioxide

Initiators, stabilizers and pigments (<1%)

Al2O3: aluminum oxide; HEMA, 2-hydroxyethyl methacrylate; K2O: potassium oxide; Li2O: lithium superoxide; MgO: magnesium oxide;
MDP: 10-methacryloyloxydecyl dihydrogen phosphate; P2O5: phosphorus pentoxide; SiO2: silicon dioxide; ZnO, zinc oxide; ZrO2: zirconium oxide.

MATERIALS AND METHODS
The materials used in the bonding procedure are listed in
Table 1.
Experiment 1: Tensile bond test
Specimen fabrication
Lithium disilicate ceramics blocks (e.max CAD, Ivoclar Viva-
dent) were used in this study. Specimens (5 mm thick x
15 mm wide x 15 mm long) were retrieved from original blocks
using a low-speed diamond saw (IsoMet, Buehler; Lake Bluff,
IL, USA) and sintered. One surface of each specimen was
ground using 600-grit silicon carbide paper under water rinsing.
The specimens were ultrasonically cleaned in deionized water
for 5 min followed by ethanol for 2 min and then air dried.
Surface preparation
The specimens were left as is or were contaminated with
human saliva. To contaminate, the specimens were im-
mersed in saliva for 1 min. Saliva was collected from one of
the authors who had refrained from eating and drinking
1.5 h prior to the collection procedure under a protocol ap-
proved by the Ethics Committee at Tokyo Medical and Den-
tal University (No. D2017-053). All experiments were per-
formed using fresh saliva collected on the same occasion.
Then excess saliva was removed by water spraying for 15 s,
followed by air drying for another 15 s.
Each group was further divided into five subgroups
(n = 20, with and without contamination) according to the
surface treatment performed:
y Control: no pretreatment.
y MP: a thin coat of Monobond Plus (MP; Ivoclar Vivadent)
was applied with a brush and the material allowed to
react for 60 s. Subsequently, any remaining excess was
dispersed with a strong air stream.
y PA+MP: surfaces were etched with 37% phosphoric acid
(PA; Total Etch, Ivoclar Vivadent) for 20 s and then
rinsed and dried. After etching, MP was applied as in the
MP group.
y HF+MP: surfaces were etched with < 5% HF (IPS Ceramic
Etcting Gel, Ivoclar Vivadent) for 20 s and then rinsed and
dried. After etching, MP was applied as in the MP group.
y MEP: MEP was applied, rubbed for 20 s, and left on the
surface for a further 40 s for sufficient reaction. It was
subsequently washed off with water and then dried with
air for another 10 s.
Tensile bond strength test
After surface treatment, a 100-μm-thick piece of aluminum
masking tape with a 4-mm diameter hole was placed on

Vol 21, No 1, 2019 53

Lyann et al
e.max CAD disks
600# SiC paper polishing
Without saliva With saliva contamination
Water HF PA ME Water
cleaning cleaning
XPS Analysis
each ceramic surface. A metal rod treated with a metal ad-
hesive primer (Alloy Primer, Kuraray Noritake; Tokyo, Japan)
was attached to each ceramic block using one of the 3
resin cements (Ivoclar Vivadent): Variolink Esthetic DC (VE),
Multilink Automix (MA), and SpeedCEM (SC). The resin ce-
ment was light cured for 40 s with a curing unit at a light
intensity of 600 mW/cm2 (Optilux 501, Demetron-Kerr; Dan-
bury, CT, USA). The cemented specimens were left to com-
plete polymerization at room temperature for 30 min, then
stored in distilled water at 37°C for 24 h. A total of 300
specimens were produced in 5 surface treatment groups
with 3 resin cements and tested under two conditions: with
or without saliva contamination (n = 10). Tensile bond
strength (TBS) was measured in a universal testing appara-
tus (Autograph-J, Shimadzu; Kyoto, Japan) at a crosshead
speed of 2 mm/min.16
Failure mode analysis
The fractured interfaces of the debonded specimens were
examined using a light microscope (OCS 912042, Olympus;
Tokyo, Japan) to calculate the debonded area and assign
failure modes. The failure modes were classified into the
following three types: type I: adhesive failure, no resin ce-
ment remnant on the ceramic block; type II: mixed failure,
fracture comprises both the ceramic block and resin ce-
ment (some ceramic and some resin cement visible); type
III: cohesive failure, fracture within resin cement, fracture
surface consists of only resin cement. Representative sam-
ples were examined in a scanning electron microscope
(SEM, JSM-5310LV, JEOL; Tokyo, Japan) with an accelera-
tion voltage of 15 KV after sputtering using a conductive
layer of gold to determine the pattern of debonding.
Statistical analysis
According to the Shapiro-Wilk test, the data were normally
distributed (p > 0.05). Therefore, TBS data in MPa were ana-
lyzed separately for each cement by two-way ANOVA, followed
54
Fig 2 Schematic illustration of specimen
preparation methods for surface analysis.
Saliva immersion for
1 min, rinsing with water
spray for 15 s, air drying
HF PA ME
by the t-test with Bonferroni correction for pairwise compari-
sons. The two factors analyzed were surface treatments and
storage conditions. For all analyses, a confidence level of
95% was assumed. All statistical procedures were performed
using SPSS software (SPSS 22, IBM; Chicago, IL, USA).
Experiment 2: Surface Analysis
The surfaces of e.max CAD disks were prepared following
the same procedure as the tensile bond strength test. Each
group was divided into four subgroups (n = 2, with and with-
out contamination) according to the surface treatment per-
formed: control, 5% HF, 37% PA, and MEP in Fig 2.
X-ray photoelectron spectroscopy (XPS) was used to ana-
lyze the surfaces of the e.max CAD samples. XPS (JPC-
9010MC, JEOL; Tokyo, Japan) analyses were performed
using a Mg Kα x-ray source under the following conditions:
operating pressure, 10−7 Pa; emission current, 10 mA; ac-
celerating voltage, 10 kV. Wide scans were measured at
pass energies of 100 eV.
RESULTS
Experiment 1: Tensile Bond Strength Test
Tables 2 to 4 show tensile bond strength results as well as
failure modes, with or without saliva contamination. The two
surface treatment factors (with or without saliva contamina-
tion and surface treatment) and their interactions were sta-
tistically significant for all the cements (p < 0.05). The typi-
cal failure modes as observed with SEM are shown in (Fig 3).
Variolink esthetic DC (VE)
In both conditions, HF+MP and MEP resulted in statistically
significantly higher mean TBS than did the control, MP, and
PA+MP (p < 0.05) (Table 2). After saliva contamination,
there were no statistically significantly differences vs
groups without saliva. Regarding failure analysis, almost all
The Journal of Adhesive Dentistry
 Lyann et al

Table 2 Tensile bond strength means and standard deviations in MPa to Variolink Esthetic DC (VE)

Surface treatment Control MP PA+MP HF+MP ME

3.5 ± 1.4abcd 25.6 ± 5.4aef 27.6 ± 4.4bgh 40.6 ± 6.3ceg 37.0 ± 6.6dfh
Without saliva
(10/0/0) (0/0/10) (0/0/10) (0/0/10) (0/0/10)

0.6 ± 0.2abcd 26.5 ± 5.1ae 26.2 ± 6.3bfg 36.7 ± 9.8cef 33.9 ± 5.9dg
Saliva contamination
(10/0/0) (0/2/8) (0/0/10) (0/0/10) (0/0/10)

All groups n = 10. Failure modes: adhesive failure/ mixed failure/ cohesive failure. Same lowercase superscript letters indicate significant differences
between the rows (p < 0.05).

Table 3 Tensile bond strength means and standard deviations in MPa to to Multilink Automix (MA)

Surface treatment Control MP PA+MP HF+MP ME

7.1 ± 0.9abcd 25.1 ± 5.8aA 31.2 ± 6.5b 29.1 ± 5.2c 26.1 ± 3.9d
Without saliva
(10/0/0) (10/0/0) (0/0/10) (4/4/2) (0/0/10)

6.9 ± 2.8abcd 16.8 ± 2.8aefgA 31.5 ± 9.7be 31.4 ± 5.1cf 26.3 ± 7.1dg
Saliva Contamination
(10/0/0) (10/0/0) (0/0/10) (9/0/1) (0/0/10)

All groups n = 10. Failure modes: adhesive failure/ mixed failure/ cohesive failure. Same lowercase superscript letters indicate significant differences
between the rows (p < 0.05). Same uppercase superscript letters indicate significant differences between the columns (p < 0.05).

Table 4 Tensile bond strength means and standard deviations in MPa to SpeedCEM (SC)

Surface treatment Control MP PA+MP HF+MP ME

5.8 ± 1.3abcd 28.2 ± 5.0aA 32.9 ± 8.7b 31.1 ± 5.5c 31.0 ± 4.7d
Without saliva
(10/0/0) (0/0/10) (0/0/10) (0/4/6) (0/0/10)

6.6 ± 3.4abc 13.2 ± 3.6defA 28.7 ± 4.2ad 27.1 ± 7.3be 31.4 ± 6.9cf
Saliva contamination
(10/0/0) (10/0/0) (0/0/10) (7/0/3) (0/0/10)

All groups n = 10. Failure modes: adhesive failure/ mixed failure/ cohesive failure. Same lowercase superscript letters indicate significant differences
between the rows (p < 0.05). Same uppercase superscript letters indicate significant differences between the columns (p < 0.05).

specimens showed cohesive failure, except the control
group, both with and without saliva contamination.
Multilink Automix (MA)
The control group presented lower bond strength at base-
line in both conditions (Table 3). Without contamination,
MP, PA+MP, HF+MP and MEP showed the highest bond
strengths. After saliva contamination, MP showed signifi-
cantly lower bond strength than did the other groups
(p < 0.05). A higher ratio of cohesive failures was observed
in groups with higher bond strengths. After saliva contami-
nation, 100% adhesive failures were noticed after no sur-
face treatment (control), MP, and HF+MP.
SpeedCEM (SC)
The control group presented the lowest bond strength at
baseline with or without saliva contamination. After saliva
contamination, no significant decrease was observed in
PA+MP, HF+MP, and MEP (p > 0.05). However, bond
strength in the MP group decreased significantly after saliva
contamination (Table 4). Regarding failure mode, MEP and
PA+MP resulted in 100% cohesive failure, while more adhe-
sive failures were observed in MP and HF+MP after saliva
contamination.
Experiment 2: Surface Analysis
The typical wide-scan spectra from XPS analysis are shown
in Fig 3. Clear N-1s and C-1s peaks were identified by XPS
analysis. After saliva contamination, the intensities of N-1s
and C-1s peaks increased. In HF, Zn-2p peaks were de-
tected under both conditions. In HF and PA, there were no
N-1s peaks and small C-1s peaks. In MEP, C-1s and F-1s
peaks were the specific peaks under both conditions, but
there was no N-1s peak after saliva contamination.

Vol 21, No 1, 2019 55

Lyann et al
a b
LD RC
LD
Fig 3 Representative SEM images (35X) of typical failure modes. A clean ceramic surface was indicative of adhesive failure between
ceramic and cement. Mixed failure showed surfaces with both ceramic and resin cement. Cohesive failure in resin cement was indicated by
resin cement particles attached to the ceramic surface. RC: resin cement; LD: lithium disilicate.
DISCUSSION
Intraoral seating of pre-etched glass ceramics during a try-in
procedure frequently results in salivary contamination, and
if this contamination is not removed, it may result in de-
creased bond strength between the resin cement and the
glass-ceramic surface. The null hypothesis was rejected, as
statistically significant differences in the tensile bond
strength of resin cement to lithium disilicate ceramic were
found based on the type of surface and cleaning proce-
dures. Etching or rinsing of the pre-etched glass-ceramic
surface after contamination is necessary to dislodge the
saliva and allow more effective bonding. The use of surface
treatments according to the manufacturer’s instructions on
an etched, saliva-contaminated lithium disilicate surface be-
fore silanization resulted in bond strengths similar to that of
the uncontaminated control group. For those clinicians
whose laboratories do not pre-etch the ceramics or who mill
their lithium disilicate restorations chairside, rinsing the sa-
liva-contaminated ceramic after try-in and then etching with
hydrofluoric acid in the operatory is adequate, as it provides
bond strengths similar to the uncontaminated control.
Saliva consists of organic materials such as salivary pro-
teins, bacteria, and food debris in an aqueous solution.
After saliva immersion, salivary protein adsorption occurs
not only on the tooth surface,2 but also on the restorative
materials.5,10 Non-covalent adsorption of salivary proteins
occurred on this surface after the immersion of ceramic
into saliva for 60 s. This organic coating could not be re-
moved by rinsing with tap water for 15 s, as shown by XPS,
revealing a considerable increase in C and N after saliva
immersion and rinsing.
Cleaning the glass-ceramic surface with only water spray
after saliva contamination resulted in significantly lower
bond strength to lithium disilicate glass ceramic compared
to the uncontaminated control group. All specimens showed
low initial bond strengths and debonded spontaneously with
100% adhesive failure at the ceramic surface. Other clean-
ing procedures led to bond strength that did not differ sta-
tistically significantly from the uncontaminated groups.
56
c
RC
The specimens bonded without silane primer in the con-
trol group had statistically significantly low TBS compared
to the other groups with or without saliva contamination.
The use of silane primer, alone or in combination with the
etchant, is clinically essential for the adhesive bonding of
lithium disilicate ceramic. The use of silane without acid
etching (MP group) resulted in lower bond strengths in com-
parison with the PA+MP or HF+MP or MEP.
To avoid the detrimental effect of saliva contamination
on resin-to-ceramic bond strength, ceramic restorations
should be etched and silanized after the try-in procedure.27
Several studies reported that phosphoric acid cleaning was
effective for saliva decontamination,21,35 whereas others
reported it to be ineffective.11,31 Acid cleaning requires
water rinsing, and the remaining water may inhibit bonding
efficacy.13 In this study, phosphoric acid cleaning did not
work as well as HF in VE resin cement; HF resulted in sta-
tistically significantly higher bond strength (40.6 ± 6.3 MPa)
than PA (27.6 ± 4.4 MPa) in VE.
Interestingly, in the present study, TBS was comparable
when resin cement was bonded to lithium disilicate ceramic
using MEP or HF+MP with all resin cements. MEP contains
trimethoxypropyl methacrylate for silanizarion and polyfluor-
ide for etching. It has been indicated that the bond between
silica and fluoride is extremely strong.17 Therefore, a pos-
sible explanation for the effective bonding of MEP to lithium
disilicate ceramic may be attributed to the chemical affinity
between silica in lithium disilicate ceramic and ammonium
tri-fluoride in MEP.28
The bond quality of ceramic restorations should not only
be assessed by bond strength measurements. Another im-
portant quality indicator is provided by the analysis of frac-
ture modes.6,14,16,25 The failure modes of the experimental
groups were investigated using a light microscope and
SEM. If adhesive failure modes occur more frequently, it
can be an indication of lower bond quality. In this study,
adhesive failure modes were observed in specimens which
were not silanized or only silanized after contamination. Co-
hesive failures (fractures within the composite resin) fre-
quently occurred in MEP. In these cases, the bond strength
The Journal of Adhesive Dentistry

Fig 4 Typical spectra of wide-scan using XPS.
Counts
1000
between the glass-ceramic surface and the composite resin
could exceed the internal strength of the composite resin.
Consequently, MEP self-etching silane primer of glass ce-
ramic surface after saliva contamination is a simple and
useful method to increase the quality of the bond.
XPS was performed to identify the contamination and the
efficacy of cleaning methods.32 According to XPS analysis,
there were no N-1s and small C-1s peaks in the control
group. However, after saliva contamination, both N and C
peaks derived from salivary proteins on the lithium disili-
cate surface were detected. In HF group, Zn-2p peaks were
detected both with and without saliva contamination. HF
formed microporosities as the glass matrices were dis-
solved, leaving ZnO exposed on that treated surface. In HF
and PA groups, N-1s was not detected and the C-1s peak
was small even with saliva contamination. This shows that
these acids were able to remove the contaminated saliva
protein on the lithium disilicate surface. MEP is partly com-
posed of trimethoxypropyl methacrylate, which leaves a thin
silane layer to chemically bond to the ceramic after water
rinsing and drying of the treated surface. Although the
mechanism of action of MEP is not fully clear, EL-Daman-
houry and Gaintantzopoulou8 found fluorine residue on the
treated ceramic surface using energy dispersive x-ray analy-
sis. In this study, C-1s and F-1s were the characteristic
peaks in both conditions. However, there was no N-1s peak
after saliva contamination. The F-1s and C-1s peaks in the
MEP group were higher than those in the other groups. A
small F-1s peak might be the results of remaining ammo-
nium polyfluoride, which mildly etched the lithium disilicate
surface to achieve the etching pattern. A C-1s peak was
also detected in the saliva contaminated group. However,
these peaks are always accompanied by an N-1s peak. C
peaks in the MEP group, however, lack corresponding N-1s
peaks both with and without saliva contamination. From
this point of view, the C-1s peak in the MEP group could be
coming from the silane coupling agent on the lithium disili-
cate surface.
Although adhesion between resin cement and etched
and silanized glass ceramics is well established, possible
Vol 21, No 1, 2019
Lyann et al
Counts
800 600 400 200 0 1000 800 600 400 200 0
Binding energy (eV) Binding energy (eV)
saliva contamination during the intraoral try-in procedures
may impair bond strengths, demonstrating the clinical sig-
nificance of this investigation particularly for minimally inva-
sive preparations which rely on retention from adhesive
bonding. Adhesive cementation protocols should consider
removal of contamination media as a critical step to im-
prove the longevity of bonded restorations. More in vitro
studies are needed to obtain further information under long-
term water storage and thermalcycling conditions after sa-
liva contamination.
CONCLUSION
Saliva contamination on the bonded surface of the lithium
disilicate glass ceramics before its cementation should be
avoided. Treating the surface with phosphoric or hydro-
fluoric acid in combination with silane coupling agent or the
use of Monobond Etch & Prime were effective methods for
removing saliva contamination and ensuring proper bonding
of the resin cement to the lithium disilicate glass-ceramic
bonding surface.
ACKNOWLEDGMENTS
We would like to thank Ivoclar Vivadent for supplying lithium disilicate
disks. This work was supported by the JPSP Grant-in-Aid for Scientific
Research (C) 17K11701 and the Cooperative Research Program of
the Institute for Catalysis, Hokkaido University (Grants #16B1004
and #17B1007).
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Clinical relevance: For adhesive cementation of lithium
disilicate glass ceramics, the newly developed Mono-
bond Etch & Prime can effectively remove saliva contam-
ination and provide bond strengths comparable to the
combination of hydrofluoric acid with Monobond Plus.
The Journal of Adhesive Dentistry