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Cleaning Zirconia Surface Prior To Bonding. A Comparative Study of Different

Methods and Solutions

Article  in  Journal of Prosthodontics · May 2021

DOI: 10.1111/jopr.13389

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Cleaning Zirconia Surface Prior To Bonding: A Comparative
Study of Different Methods and Solutions
Taiseer A. Sulaiman, DDS, PhD ,1 Ali Altak, DDS,1 Awab Abdulmajeed, DDS, MS ,2
Brandon Rodgers, BS,1 & Nathanial Lawson, DMD, PhD 3
1
Division of Comprehensive Oral Health, Adams School of Dentistry, University of North Carolina at Chapel Hill, Chapel Hill, North Carolina
2
Department of General Practice, School of Dentistry, Virginia Commonwealth University, Richmond, Virginia
3
Division of Biomaterials, University of Alabama School of Dentistry, Birmingham, Alabama

Keywords Abstract
Zirconia; salivary contamination; zirconia
cleaning; shear bond strength.
Purpose: To evaluate resin cement bond strength after removal of salivary contami-
nation from a zirconia surface using different cleaning solutions and air-borne particle
Correspondence
abrasion.
Dr. Taiseer A. Sulaiman, Division of Materials and methods: One-hundred and twenty zirconia specimens (KATANA
Comprehensive Oral Health, UNC Adams STML, Noritake) were prepared and divided into 12 groups (n = 10). Groups were
School of Dentistry, 4606 Koury Oral Health subjected to a notched-edge shear bond strength test (ISO 29022) to analyze the bond-
Sciences Building, CB 7450, Chapel Hill, NC ing efficiency of a resin cement (Panavia V5, Kuraray Noritake Dental Inc.) before
27599. and after contamination with saliva. Group 1 (control) was prepared and cemented
E-mail: [email protected] without salivary contamination. Group 2 was coated with ceramic primer (Clearfil
Ceramic Primer Plus, Kuraray Noritake Dental Inc.) then subjected to salivary con-
Accepted May 11, 2021 tamination then tested. Group 3 was contaminated, cleaned by air-borne particle abra-
sion, ceramic primer and resin cement applied, and tested. Groups 4 to 12 were con-
doi: 10.1111/jopr.13389 taminated, and then different cleaning solutions (water, 4.5% hydrofluoric acid, 35%
phosphoric acid, Ivoclean, KATANA cleaner, Zirclean, sodium hypochlorite 4%, and
7.5%) were used to decontaminate the zirconia surface, followed by ceramic primer,
resin cement application, and tested. One-way ANOVA and Tukey post-hoc analysis
was used to analyze the data.
Results: One-way ANOVA showed statistical differences among cleaning proce-
dures (p < 0.001, F = 13.48). Air-borne particle abrasion was the only group which
provided a bond strength (21 ± 2.8 MPa) that was not statistically different than the
control group in which no contamination occurred (25.3 ± 3.3 MPa) (p = 0.247). The
use of hydrofluoric acid and zirconia cleaning solutions resulted in bond strengths
values which were not statistically different from each other (17.5-19.1 MPa).
Conclusion: Air-borne particle, zirconia cleaning solutions and hydrofluoric acid
are feasible to decontaminate the zirconia surface from saliva prior to bonding the
restoration.

Zirconia restorations are becoming increasingly popular due to contaminants.2 However, remaining inorganic phosphorus (P)
their esthetic properties, strength, and ease of chairside milling. residue may limit the bond strength of resin cement to the zir-
After the fabrication of the restoration, a “try-in” is necessary conia surface.3–5 Particle abrasion using aluminum oxide (50
to evaluate the fit prior to cementation. However, salivary con- µm) is another effective method to remove contaminants from
tamination of the restoration during the try-in poses a potential ceramic surfaces.4,6 It has been considered the only method to
issue with the bond strength between the zirconia and cement.1 reliably remove contaminants and completely restore the ce-
Therefore, the surface of the restoration needs to be properly ramic surface.1,7 However, physical abrasion as a means to
cleaned of contamination to ensure sufficient bond strength and clean a ceramic surface remains controversial due to the ef-
longevity. fect it may have on the mechanical strength of the zirconia.
Phosphoric acid (37%) followed by thorough rinsing is a Although over abrading may induce large surface flaws which
common method of cleaning contaminated glass-ceramic sur- may affect strength longevity, it has been reported that particle
faces after try-in. Cleaning zirconia restorations with phospho- abrasion can increase flexural strength of conventional 3 mol%
ric acid has also been observed to successfully remove organic yttria zirconia if performed properly.8,9

Journal of Prosthodontics 00 (2021) 1–6 © 2021 by the American College of Prosthodontists 1

Cleaning Zirconia Bonding Surface Sulaiman et al

Ceramic cleaners have become an effective way to safely 50 µm aluminum oxide at 2.5 bar pressure (10 seconds) at
remove contaminants without affecting bond strength or me- 10 mm distance (Microetcher IIA, Danville Materials, San
chanical strength of the ceramic substrate. Previous studies Ramon, CA) and ultrasonically cleaned in distilled water for
have shown ceramic cleaners, such as Ivoclean (Ivoclar Vi- 2 minutes followed by drying with a stream of air. After sur-
vadent, Schaan, Liechtenstein), lead to more effective cleaning face abrasion, samples were divided into 12 groups (n = 10)
and stronger bond strengths compared to water rinsing or us- (Fig 1 Table 1) for testing. The sample size was calculated
ing phosphoric acid.5,6,10–14 The effectiveness of other ceramic using G*Power v. 3.1.9.3 (Heinrich-Heine-Universität Düssel-
cleaners such as ZirClean (BISCO, Inc., Schaumburg, IL) dorf, Germany). Input values were set as: Effect size f = 0.40,
and Katana cleaner (Kuraray Noritake Dental Inc., Okayama, α err prob = 0.05, Power (1-β err prob) = 0.80. The total sam-
Japan) remain largely unknown. According to their manufac- ple size was determined to be 120 (n = 10/group) with an ac-
turers, each cleaning solution works by a different mechanism tual power = 0.8217.
of action. Ivoclean is an alkaline cleaning solution composed In the control group (Group 1) a ceramic primer (Clearfil
of hyper-saturated zirconia particles which attracts contami- Ceramic Primer Plus, Kuraray Noritake Dental Inc., Okayama,
nants via a chemical gradient from the surface of the restora- Japan) was applied with agitation for 10 seconds using an ap-
tion. This allows the contaminants to be rinsed away with wa- plicator brush then dried for 5 seconds with a dry-air stream
ter before cementation. ZirClean cleaning gel is an alkaline prior to cement application. In Group 2, specimens were coated
non-abrasive cleaner composed of potassium hydroxide which with the ceramic primer for 10 seconds and dried, followed by
breaks the ionic bond between the contaminant and restorative contamination with human saliva spread with a microbrush for
surface. Katana cleaner is an acidic (pH 4.5) ceramic cleaner 3 minutes. Saliva used in this study was collected from a single
composed of a 10-methacryloyloxdecal dihydrogen phosphate participant and was stored in a sterile container at 4°C (up to 6
(MDP) salt which is proposed to remove contaminants intra- hours) until tested [Institutional Review Board (IRB#273921)].
orally and/or extra-orally. The hydrophobic group of the MDP Groups 3 to 12: saliva was applied to the zirconia surface and
salt bonds to the contaminant. The exposed hydrophilic phos- spread with a microbrush for 3 minutes before rinsing with wa-
phate group allows it to be rinsed away with water. Some pre- ter and drying, cleaned (different methods), then coated with
vious studies have also reported that sodium hypochlorite can the ceramic primer. In Group 3, samples were cleaned (af-
effectively clean saliva from zirconia.4,14–16 ter contamination) with water rinsing only for 20 seconds. In
Ceramic primers that contain MDP are used to treat the sur- Group 4, samples were cleaned (after contamination) using the
face prior to cementation to enhance the bond strength of zir- initial abrasion protocol. Samples were treated with 4.5% hy-
conia to the resin cement. The phosphate group of the MDP drofluoric acid (HF, Group 5) or 35% phosphoric acid (Group
bonds with the surface of the zirconia, while the methacrylate 6) for 20 seconds and rinsed with water. Samples were cleaned
end bonds the resin cement. However, it has been suggested with Ivoclean (Group 7), Katana Cleaner (Group 8) or ZirClean
to use MDP as a preventive measure against initial contami- (Group 9) according to the application instructions of the man-
nation due to the phosphate group bonding the zirconia sur- ufacturer. In Group 10, samples were cleaned with 4% sodium
face, thereby exposing the hydrophobic methacrylate ends of hypochlorite for 20 seconds without agitation and rinsed. Sam-
the monomer. The exposure of the hydrophobic ends creates ples were cleaned with 7.5% sodium hypochlorite with agita-
a boundary, preventing surface wetting by saliva. Angkasith et tion for 20 seconds (Group 11) and 60 seconds (Group 12) and
al, concluded that if an MDP primer was used prior to try-in, rinsed. Table 2 shows the composition, concentration, and pH
the surface may be cleaned with 20 seconds of water rinsing.10 of the solutions used in the study.
This study aims to evaluate the bond strength of resin cement Notched-edge shear bond strength test (NE-SBS, ISO ISO
to zirconia after cleaning the zirconia surface from saliva con- 29022) was used to evaluate bond strength to the zirconia
tamination using different cleaning methods, and to determine surface based on each cleaning method.17 Samples were cen-
any significant differences in bond strength between zirconia tered and tightened in fixtures for bond strength testing (Ultra-
cleaning solutions. The null hypotheses are that there will be dent Products Inc., South Jordan, UT). Adhesive resin-cement
no significant effect of cleaning method on the bond strength (Panavia V5, Kuraray Noritake Dental Inc., Okayama, Japan)
between resin cement and zirconia, and there will be no differ- was inserted into an opening (Ø2.3 mm) in the plastic fixture.
ence in bond strength after the use of different cleaning solu- The top-surface of the cement was polymerized for 10 sec-
tions. onds using a polymerizing light (Elipar Deepcure-S, 3M, Saint
Paul, MN) with an average power of 960 mW. The samples
Materials and methods were stored in distilled water at 37°C for 24 hours and tested.
The NE-SBS test was performed using a Universal Instron ma-
One-hundred and twenty square-shaped (10 mm × 10 mm × chine (Model 4411, Instron, Norwood, MA). After a load cali-
1.5 mm) zirconia samples (KATANA STML, Noritake Inc., bration, each sample was positioned horizontally in the testing
Okayama, Japan) were fabricated for this study. Surface finish- fixture and loaded at 1 mm/min until failure. The NE-SBS was
ing was performed using a series of silicon carbide grits (600 calculated from the peak failure load (MPa). The surface of
and 1200) at 300 rpm for 30 seconds each. Samples were then each sample was inspected under a stereomicroscope (100 ×),
sintered according to manufactures’ instruction and inspected and the failure type was recorded: adhesive, cohesive, or mixed
for any visible defects and then mounted in acrylic resin failure.
(VariDur 200, Buehler, Lake Bluff, IL) for placement within A one-way ANOVA was used to compare bond strength
the shear bond fixture. Each sample was particle abraded with values. The post-hoc tests for the pairwise differences were

2 Journal of Prosthodontics 00 (2021) 1–6 © 2021 by the American College of Prosthodontists

Sulaiman et al Cleaning Zirconia Bonding Surface

Grp1 Grp2 Grp 7 Grp 8

Grp3 Grp4 Grp 9

Grp 10

Grp5 Grp6
Grp 11 Grp 12

Figure 1 Bonding failure mode of resin cement to zirconia is “adhesive” in all groups tested.

conducted using Tukey post-hoc analysis. A p-value <0.05 nation of a zirconia surface on shear bond strength of resin
was considered statistically significant in two-tailed statistical cement to the surface. Achieving a long-lasting restoration is
tests. All analyses were conducted using SPSS. dependent upon successfully creating a reliable bond between
the tooth structure and the restorative material. Failure to de-
Results contaminate a bonding surface is a frequent cause for bond
failure.18,19 Therefore, ensuring all bonding surfaces are free of
The mean and standard deviation for each group is presented contaminants is important for the longevity of the restoration.
in Table 1. A one-way ANOVA showed statistically significant Try-in of zirconia restorations brings bonding surfaces into
differences between the shear bond strength to zirconia follow- contact with contaminants (saliva, blood, etc.) in the oral cav-
ing different cleaning methods (Table 3, p < 0.001). Significant ity. Various techniques and cleaning methods exist for remov-
differences between groups were determined with a Tukey post ing the organic contaminants and restoring the surface prior to
hoc analysis (Table 1). The only cleaning method which did cementation.
not produce a lower bond strength than the control group in Each test group was subjected to salivary contamination, fol-
which no contamination occurred was application of air-borne lowed by the corresponding cleaning method and cementation.
particle abrasion following salivary contamination (p = 0.247). The effectiveness of each cleaning method was determined
There was no significant difference in bond strength between using NE-SBS. The results showed that there was a signifi-
the designated zirconia cleaning solutions (p = 0.105) cant difference in bond strength between the different meth-
ods, thus rejecting the null hypothesis. The uncontaminated
Discussion control group (Group 1) followed manufacturer recommended
instructions for surface preparation and cementation to the zir-
The primary purpose of this study was to compare the effec- conia surface and hence it resulted in the highest bond strength
tiveness of different cleaning methods after saliva contami- (25.3 MPa). The application of a ceramic primer prior to

Journal of Prosthodontics 00 (2021) 1–6 © 2021 by the American College of Prosthodontists 3

Cleaning Zirconia Bonding Surface Sulaiman et al

Table 1 Mean (standard deviation) shear bond strength (MPa) of resin cement to zirconia

Notched-edge shear
Cleaning method bond strength (MPa)

Group 1 (Control) Ceramic primer 25.3a (3.3)

Group 2 Ceramic primer, saliva, water 13.1d (1.6)
Group 3 Saliva, water, ceramic primer 14.8c (2.6)
Group 4 Saliva, particle abrasion, ceramic primer 21.0a,b (2.8)
Group 5 Saliva, Hydrofluoric acid (4.5%), ceramic primer 19.1b,c (2.7)
Group 6 Saliva, Phosphoric Acid (35%), ceramic primer 10.0d (2.8)
Group 7 Saliva, Ivoclean, ceramic primer 17.5b,c (4.0)
Group 8 Saliva, Katana Cleaner, ceramic primer 18.6b,c (3.6)
Group 9 Saliva, ZirClean, ceramic primer 18.3b,c (3.7)
Group 10 Saliva, Sodium Hypochlorite (4%), ceramic primer 15.1c (2.3)
Group 11 Saliva, Sodium Hypochlorite 7.5% (20s), ceramic primer 14.7c (1.1)
Group 12 Saliva, Sodium Hypochlorite 7.5% (60s), ceramic primer 16.1b,c (3.3)
∗
Similar superscript letters indicate no statistical significance (p < 0.05).

Table 2 Properties of cleaning solutions used in the study 13.1 MPa) or after (Group 3, 14.8 MPa). When organic mate-
rial from the saliva comes in contact with the zirconia surface,
Solution Composition Concentration pH
ionic bonds are formed. Therefore, water alone is incapable of
Deionized Water – – 7 interacting or dissolving the salivary proteins and decontami-
HF – 4.5% 2 nating the zirconia surface.
Phosphoric Acid – 35% <1 Air-borne particle abrasion produced the highest shear bond
Ivoclean Polyethylene Glycol 2.5-10% 13 strength (21 MPa) of all tested cleaning methods, suggesting
Sodium Hydroxide ≤2.5% the most complete surface restoral. Although mechanical sur-
Katana Cleaner Triethanolamine <3% 4.5 face abrasion has been reported to be the most effective way of
Polyethyleneglycol NA decontaminating a ceramic surface, it remains a controversial
10-MDP Salt NA method nonetheless.8,20 Particle abrasion roughens the surface
ZirClean Potassium Hydroxide <10% >13 which increases the wettability and surface energy in zirconia
Sodium Hypochlorite Sodium Hypochlorite 4% 12 allowing for improved retention.8 However, particle abrasion
Sodium Hypochlorite Sodium Hypochlorite 7.5% 12
may induce deleterious effects on the mechanical properties of
∗
Data were obtained via SDS of the manufacturer. zirconia. Phark et al, examined the effects of particle abrasion
on the shear bond strength of zirconia.20 They concluded that
regardless of the particle size tested (50 and 110 µm), abra-
Table 3 One-way ANOVA table sion increased the shear bond strength. A similar study by
Özcan et al examined the effects of particle abrasion on the
Sum of squares df Mean square F Sig
biaxial flexural strength of the zirconia using the same abra-
Between groups 1545.05 11 140.46 13.48 0.000 sion parameters.9 Conversely, they concluded an increase in
Within groups 958.45 92 10.42 the biaxial flexural strength after abrasion due to an increase
Total 2503.50 103 in monoclinic phase. Although the effect of abrasion on the
mechanical properties of zirconia remains controversial, it is
an effective method for mechanically detaching the contami-
salivary contamination has been reported to protect the surface nants from the surface.
from contamination prior to try-in.10 When the ceramic primer Acidic cleaning is another method used to remove organic
is agitated on the surface of the zirconia restoration, phosphate contaminants from ceramic surfaces. In Group 5, the use of
groups bond to ZrO2 , exposing the hydrophobic methacry- HF acid produced satisfying results after rinsing with water
late ends of the amphipathic molecule. The exposure of the (19.1 MPa). HF is a highly reactive substance that is particu-
methacrylate end of the molecule creates a hydrophobic bar- larly useful in restorative dentistry. Due to the interaction be-
rier, which was postulated to inhibit surface wetting and sub- tween HF and glass, glass ceramics may be etched to enhance
sequent contamination from salivary proteins.10 However, the the bonding retention of restorations. However, this interaction
results of the present study do not concur. Possibly the surface is absent when ZrO2 and HF are in contact. Instead, HF in-
contamination present at the time of cementation may have in- teracts with the organic contaminants and dissolves them from
terrupted the hydrophobic barrier of the ceramic primer, allow- the zirconia surface.21 Phosphoric acid also reacts with organic
ing organic material to attach to the zirconia surface. Therefore, contaminants to remove them from a ceramic surface. How-
it may be concluded that rinsing with water is not sufficient ever, when phosphoric acid comes in contact with zirconia,
at removing salivary proteins from the surface of the zirconia an interaction between the ZrO2 and P occurs, leaving an in-
whether the ceramic primer was applied before try-in (Group 2, organic P residue on the surface.3 This inorganic P residue

4 Journal of Prosthodontics 00 (2021) 1–6 © 2021 by the American College of Prosthodontists

Sulaiman et al Cleaning Zirconia Bonding Surface

inhibits the resin cement from bonding to the surface of the any deterioration in bond strength due to aging may be consid-
zirconia,1,4,22 ultimately affecting the bond strength between ered as an expected outcome. The surface of each sample was
the resin cement and the zirconia surface which resulted in be- examined under 100 × magnification to identify the nature of
ing the lowest amongst all cleaning methods (10 MPa). the failure as adhesive or cohesive. Adhesive failure was ob-
Recently, the introduction of ceramic cleaners has provided served unanimously in all groups, which was expected due to
clinicians with a simple step-by-step cleaning method for the values reported of the bond strength of the resin cement to
restoring ceramic surfaces after contamination. The manufac- the zirconia (Fig 1). No further magnification or analysis was
turer advertises Ivoclean as an alkaline extraoral universal ce- required.
ramic cleaner. Ivoclean has been reported as an effective way
of restoring ceramic surfaces.10,14 Ivoclean is a solution com- Conclusion
posed of highly concentrated zirconia oxide particles which
form a concentration gradient, creating an increased affinity There are different methods to clean the zirconia surface with
for phosphate as compared to the ceramic surface. Increased air-borne abrasion appearing to be the most effective, despite
affinity in the solution removes organic contaminants from the its controversy. Designated zirconia cleaners and hydrofluo-
zirconia surface which can then be rinsed away with water. Zir- ric acid may decontaminate the zirconia surface promoting a
Clean is also an alkaline cleaner for use on zirconia and other stronger bond of the resin cement to the zirconia.
ceramic restorations after try-in. Its alkalinity is due to potas-
sium hydroxide which interrupts the ionic bond formed be- Conflict of interest statement
tween the contaminant and the zirconia surface.23 Unlike Ivo-
clean and ZirClean, Katana Cleaner is acidic (pH 4.5) which The authors deny any conflicts of interest in regard to this
allows either extraoral or intraoral application. The manufac- study.
turer advertises the product as a universal cleaner capable of
removing contamination from a wide variety of dental materi-
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