Effect of Different Cleaning Regimens on the Adhesion

of Resin to Saliva-Contaminated Ceramics

DDS, PhD,1 Bahar Elter, DDS,2 Erhan Comleko

Akn Aladag,
glu,
DDS, PhD,1 Burcu Kanat, DDS, PhD,3
4
4

Mehmet Sonugelen, DDS, PhD, Atilla Kesercioglu,

DDS, PhD, & Mutlu Ozcan,
DDS, DMD, PhD5
1

Associate Professor, Department of Prosthodontics, School of Dentistry, Ege University, Izmir, Turkey
Teaching assistant, Department of Prosthodontics, School of Dentistry, Ege University, Izmir, Turkey
3
Research assistant, Department of Prosthodontics, School of Dentistry, Ege University, Izmir, Turkey
4
Professor, Department of Prosthodontics, School of Dentistry, Ege University, Izmir, Turkey
5
Professor, Clinic for Fixed and Removable Prosthodontics and Dental Materials Science, Dental Materials Unit, Center for Dental and Oral

Medicine, University of Zurich,

Zurich, Switzerland
2

Keywords
Zirconia; saliva contamination; cleaning paste;
sodium hypochlorite; glass ceramics.
Correspondence
Department of Prosthodontics,
Akn Aladag,
School of Dentistry, Ege University, Bornova
35100-Izmir, Turkey.
E-mail: aladag.a@gmail.com
The authors deny any conflicts of interest.
Accepted December 27, 2013
doi: 10.1111/jopr.12170

Abstract
Purpose: The aim of this study was to evaluate the influence of different cleaning
regimens on the microshear bond strength (SBS) of three different all-ceramic
surfaces after saliva contamination.
Material and Methods: Cubic ceramic specimens (3 3 3 mm3 ) were prepared from three types of ceramics: zirconium dioxide (Z), leucite-reinforced glass
ceramic (E), lithium disilicate glass ceramic (EX; n = 12/subgroup). A total of 144
composite resin cylinders (diameter: 1 mm, height: 3 mm) were prepared. Three
human-salivacontaminated surfaces of ceramic specimens were cleaned with either
water spray (WS), with 0.5% sodium hypochlorite solution (HC), or with a cleaning
paste (CP). Control surface (C) was not contaminated or cleaned. Composite cylinders
were bonded to each surface with a resin luting cement. All specimens were stored at
37 C in deionized water until fracture testing. SBS tests were performed in a universal testing machine (0.5 mm/min), and the results (MPa SD) were statistically
analyzed (two-way ANOVA, Bonferroni a = 0.05). Fractured surfaces were analyzed to identify the failure types using an optical microscope at 50 magnification.
Two representative specimens from all groups were examined with scanning electron
microscopy.
Results: SBS test results were significantly affected by the saliva cleaning regimens
(p = 0.01) and the ceramic types (p = 0.03). The interaction terms between the
ceramic type and saliva cleaning regimen were also significant (p < 0.05). There
were no significant differences among the SBS values (MPa SD) for the Z group
(C = 17.5 8.8; WS = 16.0 4.9; HC = 17.6 5.8; CP = 16.6 7.5; p > 0.05).
In the EX group, C resulted in significantly higher SBS values (32.6 7.4) than CP
(17.4 8.9), WS (15.6 7.3), and HC (14.3 4.5) (p < 0.05); however, C (20.4
7.1) and HC (19.2 7.5) showed higher SBS values than CP (13.8 4.8) and
WS (10.9 5.7) in the E group. Some cohesive failures within the luting resin were
observed in the E and EX groups, whereas only adhesive failures were seen in zirconia
groups for all surface treatments.
Conclusions: Different ceramic surface cleaning regimens after saliva contamination of the zirconium dioxide revealed SBS similar to the control group, whereas all
surface cleaning regimens tested significantly decreased the bond strength values in
the lithium disilicate glass ceramic. The leucite-reinforced glass-ceramic group benefited from 0.5% sodium hypochlorite solution cleaning with increased bond strengths.
Clinical significance: Adhesive cementation of zirconia presents a clinically challenging protocol, and the cementation surface contamination of the zirconia restorations
and the inadequate removal of the contaminants increase the risk of failure, as for
all ceramic types. This study demonstrated that surface cleaning regimens should be
applied according to different ceramic properties.

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Effect of Cleaning Regimens on Saliva-Contaminated Ceramics

Cementation of all-ceramic restorations by adhesive luting

resins has become a routine procedure for clinical use, and
problems in bonding of luting resins to ceramics have been
significantly solved in recent years. The success of longterm resin bond to all-ceramic restorations have been well
documented.1,2
Zirconium dioxide (zirconia) polycrystalline materials, also
called oxide ceramics, have been used in a wide range for
single and/or multi-unit fixed dental prostheses as well as implant abutments, due to their biocompatibility and relatively
high esthetic properties.3 Although adhesive cementation is
not a prerequisite for zirconia restorations,1 it is recommended
as in other all-ceramic materials in terms of decreasing the
risk of secondary caries development by sealing the impurities
around the finish line and increasing the fracture resistance of
the restored teeth and restorations.4 However, because zirconia
does not contain a silicate phase, it cannot be adhesively luted
as in silica-based all-ceramics.2 Silica-based all-ceramics have
the advantage of successful bonding with self-, light-, or dualcuring resin-luting cements to teeth provided that the luting
surfaces of such restorations are etched with hydrofluoric acid
followed by silanization,5 which has been a widely accepted
protocol; however, adhesive cementation of zirconia restorations has been best practiced by airborne particle abrasion of
the intaglio surfaces of the zirconia followed by application
of phosphate-bonded-monomercontaining composite resins.6
However, air abrasion might induce surface defects on zirconia, reducing its strength.7 Alternative luting surface conditioning methods such as selective infiltration etching, zirconia
ceramic powder coating, ceramic pearl layer application, glaze
layer application or recently introduced nanostructured alumina
(Al2 O3 ) coating might help overcome the problems occurring
due to air abrasion.8,9 Luting of zirconia restorations by conventional bis-GMA containing resin cements, which do not contain the bifunctional phosphate-bonded monomer, alone have
not been successful in establishing a durable long-term bond to
oxide ceramics.9,10
In addition to the abovementioned difficulties in achieving a
strong bond between the zirconia restoration and resin luting
cements, the try-in procedure of all-ceramic and/or zirconia
restorations causes the intaglio bonding surface of the restoration to be generally contaminated with saliva, blood, or fitting
indicator remnants such as silicone or try-in pastes, making the
adhesive cementation of the zirconia restorations even more
difficult. Failure to remove fluids or try-in materials results
in reduction of the bond strength.9,11 Thus, any inorganic or
organic contaminants should be eliminated before adhesive cementation. Commonly used methods of decontaminating the
luting surfaces of ceramic/zirconia restorations are scrubbing
the surface with acetone, application of 37% phosphoric acid
for 60 seconds once or for 30 seconds twice, immersing in
70% isopropanol for 2 minutes, cleaning with 96% ethanol
for 15 seconds, airborne-particle abrasion, 2% chlorhexidine or
5% sodium hypochlorite application, or water spray (WS).12,13
Recently, an alternative universal paste for extraoral cleaning
of pretreated ceramic and metal restoration surfaces that have
been contaminated during intraoral try-in has been developed.14
This cleaning paste (CP) consists of an alkaline suspension of
zirconium dioxide particles deemed to absorb the phosphate
2

contaminants to bond to them rather than to the surface of the

ceramic restoration, leaving behind a clean surface.13,15
Saliva contains organic materials such as salivary proteins,
enzymatic molecules, bacteria, and food debris, and inorganic
compounds, such as mineral ions, in water solution.13 Adhesion
of salivary proteins to dental materials and tooth surfaces (saliva
contamination) results in formation of acquired enamel pellicle, which is free of bacteria of 10 to 20 nm thickness within
a few minutes.16 When the protein transmission from saliva
increases, the thickness of the proteinaceous layer reaches 100
to 1000 nm between 30 and 90 minutes.17 It is almost impossible to avoid saliva contamination of all-ceramic and/or
zirconia restorations during the try-in procedure. During adhesive cementation procedures, contaminant removal plays an
important role in the durable adhesion and clinical performance
of the restoration.9,13
Therefore, the objective of this in vitro study was to evaluate
the influence of various surface cleaning regimens on microshear bond strength (SBS) of three all-ceramic surfaces after
saliva contamination, thereby suggesting a preference for a purifying procedure for all-ceramic surfaces. The null hypothesis
was that SBS values obtained with different saliva decontamination methods would not be affected by surface cleaning
regimens or different ceramic types.

Materials and methods

The brand names, types, manufacturers, chemical compositions, and batch numbers of the materials used in this study are
listed in Table 1.
Specimen preparation

Cubic specimens (3 3 3 mm3 ; N = 36) were prepared from

three types of ceramics, namely, presintered yttrium-stabilized
zirconium dioxide (IPS e.max ZirCAD; Z), leucite-reinforced
glass-ceramic (IPS Empress CAD; E), and lithium disilicate
glass-ceramic (IPS e.max CAD; EX; n = 12/subgroup) by sectioning under water cooling with a slow-speed diamond saw
(Isomet 1000, Buehler, Lake Bluff, IL). The thickness of the
saw for all groups in addition to 20 to 25% sintering shrinkage
of the zirconia for Z group was taken into consideration when
fabricating specimens in a 3 3 3 mm3 final dimension. The
presintered zirconia specimens were then sintered (InFire HTC
speed; Sirona Dental Systems, GmbH, Bensheim, Germany)
according to the manufacturers firing instructions, whereas
the lithium disilicate specimens were sintered in the furnace
(Programat P300; Ivoclar Vivadent) to convert the crystalline
intermediate (metasilicate) stage of the ceramic into the disilicate phase and to improve the flexural strength of the ceramic.
Surfaces of all specimens were wet-polished first with 800grit followed by 1200-grit silicon carbide paper for 120 seconds.
All specimens were ultrasonically cleaned (Quantrex 90 WT;
L&R Manufacturing, Inc., Kearny, NJ) in 99% ethanol for 15
minutes. All conditioning, cleaning, and bonding procedures
were carried out by the same operator. Although airborneparticle abrasion with 50 m Al2 O3 at 2.5 bar pressure was
applied on the all specimens for 15 seconds from a distance of
10 mm,15,18 glass-ceramic specimens were further etched with
R

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Effect of Cleaning Regimens on Saliva-Contaminated Ceramics

Table 1 Chemical compositions of the materials used

Product

Type

IPS e.max ZirCAD (Z)

Zirconium dioxide framework

IPS e.max CAD (EX)

Lithium disilicate veneering

ceramic block

IPS Empress CAD (E)

Leucite glass ceramic block

Ivoclean

Extraoral cleaning paste

MonoBond Plus

Universal primer mediating a

bond between metal,
glass/oxide ceramics and
resin

Variolink II

Dual-curing resin cement

Heliobond

Base

Catalyst

Tetric EvoFlow

Composite resin

Chemical composition
87% to 95% ZrO2, 4% to 6%
Y2 O3, 1% to 5% HfO2, 0% to
1% Al2 O3, < 0.2% other
oxides
57% to 80% SiO2, 11% to 19%
Li2 O2, 0% to 13% K2 O, 0% to
11% P2 O5, 0% to 8% ZrO2,
0% to 5% Al2 O3, 0% to 5%
MgO, 0% to 8% coloring
oxides
60% to 65% SiO2, 16% to 20%
Al2 O3, 10% to 14% K2 O,
3.5% to 6.5% Na2 O, 0.5% to
7% other oxides, 0.2% to 1%
pigments
10% to 15 zirconium oxide,
65% to 80% water, 80% to
10% polyethylene glycol, <1
sodium hydroxide, 4% to 5%
pigments, additives
50% to 100% ethanol, <2.5%
3-trimethoxysilylpropylmethacrylate, <2.5%
methacrylated phosphoric
acid ester

Bis-GMA, triethylene
glycoldimethacrylate,
initiators, stabilizers
Bis-GMA, TEGDMA, urethane
dimethacrylate (UDMA),
inorganic filler, ytterbium
trifluoride, initiator, stabilizer
Bis-GMA, TEGDMA, UDMA,
inorganic filler, ytterbium
trifluoride, benzoyl peroxide,
stabilizer
Bis-GMA, UDMA, decandioldimethacryate, barium glass
filler, ytterbium trifluoride,
highly dispered silica, mixed
oxide, prepolymers, additives,
catalysts, stabilizers, and
pigments

a 9% hydrofluoric acid (Ultradent Porcelain Etch; Ultradent

Products Inc., South Jordan, UT) for 60 seconds and 20 seconds for leucite (E) and lithium disilicate (EX) glass-ceramics,
respectively. All specimens were further ultrasonically cleaned
in 99% ethanol for 10 minutes.
Surface cleaning regimens

Three surfaces of each cubic ceramic specimen were contaminated with fresh human saliva obtained from a healthy female

Manufacturer

Batch number

Ivoclar Vivadent; Schaan,

Liechtenstein

S06538

Ivoclar Vivadent; Schaan,

Liechtenstein

S08650

Ivoclar Vivadent; Schaan,

Liechtenstein

P50773

Ivoclar Vivadent; Schaan,

Liechtenstein

P66483

Ivoclar Vivadent; Schaan,

Liechtenstein

P41360

Ivoclar Vivadent; Schaan,

Liechtenstein

632325

Ivoclar Vivadent; Schaan,

Liechtenstein

R71123

Ivoclar Vivadent; Schaan,

Liechtenstein

R82387

donor who had not consumed any food or drinks 1.5 hours
before sample collection18 by a cotton pellet. One surface of
each cubic ceramic specimen was used as control. Because
four of the six surfaces of each cubic specimen were used for
experimental and control groups for standardization, contamination of the surfaces to be treated was avoided using a
polyethylene mold with a square (3 3 mm2 ) window that
fit precisely to the specimens. The saliva was applied, left for
10 minutes, and then the saliva-contaminated surfaces for all
specimens were randomly divided into three groups and cleaned

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with different regimens of WS, 0.5% sodium hypochlorite solution (HC), and a CP.
Water spray: The saliva-contaminated surfaces of all specimens were washed with WS for 20 seconds, and then dried for
20 seconds.
Sodium hypochlorite solution (HC): The second salivacontaminated surface of all specimens were cleaned with 0.5%
sodium hypochlorite solution for 20 seconds, washed and rinsed
for 10 seconds, and dried for 5 seconds.
Cleaning paste: The third saliva-contaminated surface of all
specimens was rinsed with WS and dried with oil-free air. A
CP (IvocleanTM ; Ivoclar Vivadent) was applied for 20 seconds
using a microbrush, then thoroughly rinsed and dried.
Control surface (C): The untreated fourth surfaces of all specimens served as the control group.

Figure 1 Custom-made specimen holder for the application of SBS

test.

Bonding procedures

The composite resin material (Tetric EvoFlow; Ivoclar Vivadent; N = 144) was filled in a glass cylinder tube with an
inner diameter of 1 mm and photopolymerized (Bluephase G2;
Ivoclar Vivadent) from all sides for 40 seconds. After removal
from the tube, the cylindrical specimens were sectioned to a 3
mm height under water cooling with a slow-speed diamond saw.
The composite resin specimens were ultrasonically cleaned in
ethanol for 15 minutes. Polyethylene plates with a hole (diameter: 1 mm) in the center were used for preparation of the
bonding area. The ceramic surfaces, which were cleaned with
different regimens, were silanated (Monobond Plus; Ivoclar
Vivadent) using a microbrush, left 60 seconds for its reaction, and dried for 10 seconds. The bonding agent (Heliobond;
Ivoclar Vivadent) was applied with a microbrush and gently air
thinned. The resin luting cement including base and catalyst
pastes (Variolink II; Ivoclar Vivadent) was mixed according to
manufacturers instructions and applied to the ceramic surface,
which was visible from the polyethylene mold. Cleaned ceramic
surfaces and conditioned composite specimens were bonded,
excess resin was removed using a microbrush, and the surfaces
were photopolymerized for 40 seconds from each aspect of
the specimens. After polymerization, polyethylene molds were
gently removed, and the specimens were stored in deionized
water at 37 C for at least 48 hours until fracture testing.
SBS test and failure analysis

The specimens were inserted in a custom-made specimen

holder (Fig 1) and SBS tests were performed in a universal testing machine (Autograph AG-50 kNG; Shimadzu, Kyoto, Japan) at a 0.5 mm/min crosshead speed. The shear force
was applied to the ceramic-composite interface until fracture
occurred. After SBS tests, all debonded specimens were analyzed to identify the failure types using an optical microscope
(MP 320; Carl Zeiss, Jena, Germany) at 50 magnification. After all specimens were evaluated, failure modes were classified
either as adhesive failure between the ceramic and resin (A) or
cohesive failure within the luting resin or in the composite resin
(C).19
Two representative fractured surfaces from each group and
failure type were dried by vacuum dessication and carbon
coated. A scanning electron microscope operating at 20 kV
4

(JSM-5200; JEOL, Tokyo, Japan) was used to observe the failure modes of the debonded ceramic specimens after SBS
testing.
Statistical analysis

The obtained results (MPa SD) were statistically analyzed

(SPSS 16.0 for Windows; SPSS Inc., Chicago, IL) within ceramic groups for comparison of cleaning regimens using twoway ANOVA, Bonferroni correction. Note that p < 0.05 were
considered to be statistically significant in all tests. Weibull
statistical analysis (MINITAB Version 14; State College, PA)
was applied to describe SBS analysis and to evaluate the reliability of cleaning regimens of saliva from different ceramics. The adjusted Anderson-Darling goodness-of-fit with 95%
CI estimation method of maximum likelihood was carried
out for mechanical test results data to determine the Weibull
distribution.

Results
SBS results were significantly affected by the saliva cleaning regimens (p = 0.01) and the ceramic types (p = 0.03;
two-way ANOVA). The interaction terms between the ceramic
type and saliva decontamination method were also statistically
significant (p < 0.05).
There were no significant differences among the SBS values for cleaning regimens in the Z group (p 0.05). In
the EX group, C resulted in significantly higher SBS values than CP, WS, or HC (p < 0.05); however, C and HC
showed higher SBS values than CP and WS in the E group
(Table 2).
Estimates of the parameters of the Weibull distribution
for the different ceramic groups in different decontamination methods are presented in Table 3. The test to estimate
shape parameters (p 0.05) indicated no statistical differences in Weibull shape parameters among the ceramic groups,
whereas the test for equal scale parameters (p < 0.05) indicated that ceramic types in C and HC groups had different
scale parameters for the SBS mechanical test. According to
the analysis with the Weibull distribution, probability plot and

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Table 2 SBS (MPa) results of three ceramics after application of water spray (WS), sodium hypochlorite solution (HC), and cleaning paste (CP)
cleaning regimens following saliva contamination and noncontaminated control group. Same superscript small letters indicate no significant difference
in the row, same superscript capital letters indicate no significant difference in the column. Results of two-way analysis of SBS of ceramic types
and saliva cleaning regimen (p < 0.05)
Ceramic types

E
EX
Z

Control (C)

Water spray
(WS)

Sodium hypochlorite
solution (HC)

Cleaning paste (CP)

20.4 7.1b,A
32.6 7.4b,B
17.5 8.8a,A

10.9 5.7a,A
15.6 7.3a,A
16.0 4.9a,A

19.2 7.5b,A
14.3 4.5a,A
17.6 5.8a,A

13.8 4.8a,A
17.4 8.9a,A
16.6 7.5a,A

Table 3 Relation of the scale and shape parameters among the saliva contamination methods. Different superscript letters indicate significant
differences among groups
Scale (MPa)
C

WS

HC

CP

E
EX
Z
E
EX
Z
E
EX
Z
E
EX
Z

95% CI (scale; N)

23
36b
20a
12c
18c
18c
22d
16e
20f
15g
20g
19g

Shape
a

(19, 27)
(31, 40)
(15, 26)
(9, 16)
(14, 23)
(15, 21)
(17, 27)
(14, 18)
(16, 23)
(13, 18)
(15, 26)
(15, 24)

3.5
4.8b
2.3a
2.1c
2.4c
3.8c
2.8d
3.9d
3.3d
3.7e
2.2e
2.5e

95% CI (shape)

AD

(2.2, 5.6)
(3.2, 7.3)
(1.4, 3.6)
(1.3, 3.4)
(1.5, 3.9)
(2.4, 5.9)
(1.9, 4.1)
(2.5, 6.2)
(2.2, 5.0)
(2.2, 6.1)
(1.4, 3.4)
(1.6, 3.7)

1.380
1.518
1.387
1.522
1.433
1.459
1.488
1.416
1.416
1.735
1.339
1.378

Table 4 Failure types per test group. Adhesive failure at the interface between ceramic and luting resin (A); cohesive failure within the resin only (C)
Hypochlorite
solution (0.5%)

Leucite-reinforced glass ceramic (E; n: 12)

Lithium disilicate glass ceramic (EX; n: 12)
Zirconium dioxide (Z; n: 12)

Water
spray

Cleaning
paste

Control

10
10
12

2
2
0

12
12
12

0
0
0

12
11
12

0
1
0

10
8
12

2
4
0

parametric survival plot graphics of SBS test can be seen in

Figure 2.
Mainly adhesive failures were observed for C, WS, HC,
and CP groups for all-ceramic groups; however, some cohesive failures within the luting resin were observed in E and
EX groups, while no cohesive failures were seen in zirconia
groups for C, WS, HC, and CP surface treatments (Table 4).
For the control group of zirconia specimens, a clean surface
texture of the polycrystalline structure was observed (Fig 3),
while lower amounts of surface contaminants were present in
the experimental group (Fig 4). The etched surfaces in the glass
ceramic (E) group were observed as wide grooves (Fig 5),
and HC groups revealed similar clean surfaces (Fig 6). In the
EX control group (Fig 7), the etched surfaces revealed smaller
grooves with homogenous irregularities while the experimental groups, especially CP, presented remnants on the surface
(Fig 8).

Discussion
The performance of different ceramic surface cleaning regimens with leucite-reinforced glass-ceramic, lithium disilicate
based ceramic, and zirconia specimens after human salivary
contamination has been investigated in this study. A significant
effect of the decontamination methods was observed, compared
to the control group, and ceramic types affected the SBS values. Thus, the null hypothesis was rejected.
Cleanliness of the bonding surfaces has an influence on the
success of the durable bond strength.9,20 Therefore, removal
of the saliva contaminants that occur during the try-in procedures from ceramic inner surfaces before adhesion plays an
important role in the longevity of the restorations.21 Solid substrates such as enamel, dentine and different types of restorative materials (glass ceramics and zirconia) in the oral cavity
have different polarities and physical properties, which affect

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Aladag et al

Figure 2 Survival and probability plots of different cleaning methods.

the adhesion of the salivary proteins.22 When the restoration

comes into contact with saliva during the try-in phase, an
immediate proteinaceous layer composed of adsorbed proteins,
several enzymes, glycoproteins, and other macromolecules is
formed.23,24 Through the physicochemical interactions between
the solid substrates and saliva, supramolecular protein assemblies (proline-rich proteins, PRPs) may precipitate and adhere
to the substrates by forces with different ranges.25,26 It has also
been demonstrated through X-ray photoelectron spectroscopic
(XPS) analysis that adsorption of the salivary proteins to the
zirconia surface increases the carbon, nitrogen, and silica levels, leading to an alteration in the composition of the surface.20

Therefore, immediate elimination of these precipitates is crucial for adhesion.

Although standard airborne particle abrasion was not used
as a ceramic decontamination method in this study, all-ceramic
surfaces were air abraded with 50 m Al2 O3 at 2.5 bar pressure,
simulating the as-arrived restoration from the laboratory to the
clinic, and the contamination was then conducted mimicking
the final intraoral try-in of the restoration before cementation,
and the most practical and commonly used decontamination
methods were then applied. As has been previously reported,
airborne-particle abrasion produces the surface roughness necessary for adhesive luting. On the other hand, it might increase

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the possibility of contamination and prevent adequate decontamination because of the created pits and irregularities on the
luting surfaces of the restorations.27 After the contamination
of this roughened surface by saliva, further application of air
abrasion for cleaning of the adherent surface of the restoration
might induce surface defects on zirconia, reducing its strength.7
Various methods, either tribochemical silica coating followed
by the application of the trialkoxysilane coupling agents28,29 or
airborne Al2 O3 particle abrasion followed by phosphate ester
monomer-containing primers,30 have been used to obtain good
adhesion between zirconia and resin cement. While air abrasion roughened and increased the wettability of zirconia,31 the
primers/silanes that consist of adhesive functional monomer
applications such as methacrylate phosphoric ester32 and 10methacryloyloxydecyl dihydrogen phosphate obtain the chemical bonding.33 The organophosphate monomers contain both
polymerizable functional groups, which copolymerize with the
matrix of the acrylate-based dental resin cements, or composites and phosphoric acid (phosphate ester) groups, which
bond chemically to metal oxides at the zirconia ceramic surface with Van der Waals forces or hydrogen bond.28 For this
intermolecular binding to be effective, the surfaces should
be extremely clean. Besides these advantages of phosphatebonded monomers, it was found that application of either phosphate ester containing primer or resin cement might be successful to improve the bond strength with respect to using both
of them.34,36 In this study, the zirconia surfaces were conditioned with a methacrylated phosphoric acid ester containing
universal primer (Monobond Plus) before bonding with a resin
cement.
Saliva contamination could be cleaned with several regimens;
however, limited literature has been found about the most effective method to remove the remnants from the inner surface
of the various types of ceramics. In a previous study where
the effect of contaminations (saliva and disclosing agent) and
cleaning regimens on bonding to zirconia had been investigated
using XPS chemical analysis and tensile strength testing, contamination with saliva significantly decreased the bond strength
of zirconia, and airborne-particle abrasion was the most effective cleaning regimen with respect to water rinsing, isopropanol,
and phosphoric acid gel.27 Phosphoric acid has previously been
proposed as a zirconia surface cleaning agent with the assumption that it was a good organic solvent; however, an earlier
study demonstrated that H3 PO4 led to a decrease in the bond
strength.4 In this study, 0.5% sodium hypochlorite solution
and a CP were preferred because of the lack of information
about the surface cleaning of saliva-contaminated ceramics using these materials. Sodium hypochlorite is a nonspecific proteolytic agent capable of removing the organic material and
proteins from the smear layer.37 The universal paste used in
this study is an alkaline suspension of zirconium dioxide particles in water, and it has been reported to absorb the phosphate contaminants in the media, leaving a clean surface.14 All
zirconia groups exhibited insignificant differences in terms of
bond strength values for various surface cleaning regimens;
however, SEM images (Figs 3 and 4) revealed more or less
amounts of contaminated surfaces for zirconia specimens. This
might be an explanation for high initial bond strength values
for all bonded specimens because an adhesive, from a chemi-

Effect of Cleaning Regimens on Saliva-Contaminated Ceramics

Figure 3 SEM image (5000) of the zirconia material in the control

group. A clean polycrystalline structure of the zirconia can be observed.

Figure 4 SEM image (5000) of the zirconia groups after the cleaning
paste (Ivoclean) application. The remnants on the contaminated surface
are indicated with arrows.

cal aspect, attaches well to even contaminated and/or modified

surfaces initially, but the deterioration of the bond is compromised in the short run. Thus, long-term clinical results should
be obtained for a valid cleaning and adhesion protocol to be
defined. Therefore, the abovementioned phosphate absorbing
mechanism of the universal CP used in this study might not
have completely affected the removal of PRPs in the saliva,
and thereby might have blocked the removal of these proteins
from the air-abraded and saliva-contaminated zirconia surface,
leaving behind a possible film layer. The differences among the
tested decontamination methods for the zirconia surface were
insignificant in this study. Therefore, even the most practical
WS cleaning of the zirconia surface can be recommended for
chairside cleaning procedures.
In this study, some commonly used glass ceramics besides
zirconia were tested in terms of chairside cleaning after saliva
contamination. When glass ceramics are concerned, it can be
assumed that re-etching of the previously HF acid-etched surfaces would work well for cleaning. Klosa et al15 reported that
re-etching with hydrofluoric acid was the most successful
method for cleaning the saliva-contaminated lithium disilicate ceramics (IPS e.max Press) with respect to 37%

C 2014 by the American College of Prosthodontists

Journal of Prosthodontics 00 (2014) 110 

Effect of Cleaning Regimens on Saliva-Contaminated Ceramics

Figure 5 SEM image (3000) of the leucite-reinforced ceramic in the

control group. The wider porous structure was observed after etching
with HF acid when compared to etched lithium disilicate ceramic.

phosphoric acid, 5% hydrofluoric acid, 96% isopropanol, or

an air-polishing device with sodium bicarbonate; however, repeated HF acid etching of the glass-ceramic surfaces may lead
to weakening of the ceramic structure, thus decreasing bond
strengths.38 While cleaning with 0.5% sodium hypochlorite
solution affected the SBS of saliva-contaminated, leucitereinforced glass-ceramic groups, all the decontamination methods applied in this study were found to be ineffective for
the lithium disilicate surface cleaning, SBS tests also supported these findings. As lithium disilicate ceramics contain
quartz, lithium dioxide, phosphor oxide, alumina, potassium
oxide, and other components, the block form of lithium disilicate glass-ceramic material, suitable for CAD/CAM applications, has a two-crystalline phase (metasilicate and fully crystallized lithium disilicate forms) microstructure (Li2 Si2 O5 ).14
When the glass ceramics are etched with hydrofluoric acid,
a chemical reaction: 4HF+SiO2 > SiF4 +2H2 O occurs, because the affinity of fluoride to silicon is higher than to oxygen, and microgrooves and irregularities can be formed on
the glass-ceramic surface to promote micromechanical adhesion with resin cement; however, the etchability of leucitereinforced and lithium disilicate ceramics differs due to their
chemical compositions.40 The same concentration and application time for HF acid results in higher surface roughness
in the lithium disilicate based glass ceramics when compared
with leucite-reinforced glass ceramic.41,42 Although the specimens in both glass-ceramic groups were HF acid etched according to manufacturers instructions (E: 60 seconds, EX:
20 seconds), different etching patterns were observed in the
EX and E groups, with the E group revealing a wider porous
structure easing the removal of the contaminants (Fig 5) while
in the EX group the grooves were more dense, not allowing
for the removal of remnants and saliva (Fig 7) when SEM
images were observed. The increased SBS values in the
HC group in E and decreased values in EX may stem from
the abovementioned surface mechanism. A possible explanation for the decreased SBS and increased adhesive failure
could be that an invisible thin residual organic film might
have covered the fitting surfaces of the restoration blocking
8

Aladag et al

Figure 6 SEM image (3000) of the HF acid etched leucite-reinforced

glass ceramic after cleaning with 0.5% sodium hypochlorite solution.
The wider grooves are seen as clean surfaces.

Figure 7 SEM image (3000) of the HF acid etched lithium disilicate

ceramic in the control group with more dense grooves than leucite-based
glass ceramic.

the penetration of the silane and luting cement into the

microporosities.
In correlation with SBS values, mainly adhesive failures
were observed in glass-ceramic groups for CP, WS, and HC
cleaning regimens, which related to lower bonding due to not
being effective enough to remove the saliva contaminations.
Cohesive failures within the cement observed in C indicated
a cleaner surface, which leads to higher SBS values. SEM
images of this study revealed that surface contaminants were
present in the experimental zirconia groups. A clean polycrystalline structure of the zirconia of the control group was observed (Fig 3), while the CP was unable to eliminate the surface contaminants completely (Fig 4). Cleaning with a 0.5%
hypochlorite solution proved to be effective in the E group
(Fig 6), revealing similar images in the control group (Fig 5) as
supported by SBS values. In SEM images of the EX control
group, acid-etched porous structure was observed (Fig 7), while
a clearly visible remnant layer was observed in EX-CP group,
verified by SBS (Fig 8).

C 2014 by the American College of Prosthodontists

Journal of Prosthodontics 00 (2014) 110 

Aladag et al

Effect of Cleaning Regimens on Saliva-Contaminated Ceramics

3. The use of 0.5% hypochloride on acid-etched leucite

glass-ceramic surfaces recovered the decreased SBS
values.

Acknowledgments
The authors of the study would like to thank Prof. Dr. Tijen
Pamir from the Restorative Dentistry Department, Ege University, School of Dentistry for conducting the SBS tests and
Prof. Dr. Bilge Hakan Sen from the Endodontics Department,
Ege University, School of Dentistry for her assistance with the
SEM analyses.

Figure 8 SEM image (3000) of the lithium disilicate ceramic with visible remnant layer followed by the cleaning paste application.

Although aging procedures may be required for in vitro adhesion testing of dental substrates and inorganic materials (i.e., ceramics, composites), various low-temperature aging treatments
have proven not to negatively affect the flexural strengths of
Y-TZP ceramic specimens, one of the materials tested in this
study.43-45 In another study, zirconia specimens were placed
in saline solution at 508 C and 958 C for 3 years and in distilled water at 1218 C for 2000 hours, and they did not exhibit any changes in flexural strength, even after 30 months of
low-temperature degradation treatment.46 Therefore, because
no dental substrate (dentin or enamel) was used, and the aim
was to test the effectiveness of surface cleaning regimens before luting, no artificial aging procedures were performed in
this study.
One limitation of this study was that a chemical analysis
such as XPS was not used to observe to what extent the contamination reached the irregularities and contaminated ceramic
surfaces and the amount of the removal of the contaminant.
Rather, the main objective focused on the effectiveness of the
newly developed universal CP in terms of bond strength and
electron microscopic observation of any contaminant present on
the ceramic surfaces. Further studies on the cleaning effectiveness of the most commonly preferred surface decontaminants
on conditioned real ceramic restorations ready for adhesive
cementation, but intraorally tried for final control should be
conducted, although standardization of contaminants are difficult for clinical studies, and production of duplicate ceramic
restorations may not be practical and economical.

Conclusions
From this study, the following could be concluded:
1. Different ceramic surface cleaning regimens after saliva
contamination of the zirconium dioxide revealed similar
SBS as the control group. Cleaning the surface with
WS can be recommended as a practical clinical method.
2. The use of hypochloride or CP on the acid-etched lithium
disilicate glass-ceramic surfaces after saliva contamination could not restore the decreased SBS values.

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