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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: sulaiman@unc.edu 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
their esthetic properties, strength, and ease of chairside milling.
After the fabrication of the restoration, a “try-in” is necessary
to evaluate the fit prior to cementation. However, salivary con-
tamination of the restoration during the try-in poses a potential
issue with the bond strength between the zirconia and cement.1
Therefore, the surface of the restoration needs to be properly
cleaned of contamination to ensure sufficient bond strength and
longevity.
Phosphoric acid (37%) followed by thorough rinsing is a
common method of cleaning contaminated glass-ceramic sur-
faces after try-in. Cleaning zirconia restorations with phospho-
ric acid has also been observed to successfully remove organic
contaminants.2 However, remaining inorganic phosphorus (P)
residue may limit the bond strength of resin cement to the zir-
conia surface.3–5 Particle abrasion using aluminum oxide (50
µm) is another effective method to remove contaminants from
ceramic surfaces.4,6 It has been considered the only method to
reliably remove contaminants and completely restore the ce-
ramic surface.1,7 However, physical abrasion as a means to
clean a ceramic surface remains controversial due to the ef-
fect it may have on the mechanical strength of the zirconia.
Although over abrading may induce large surface flaws which
may affect strength longevity, it has been reported that particle
abrasion can increase flexural strength of conventional 3 mol%
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
Ceramic cleaners have become an effective way to safely
remove contaminants without affecting bond strength or me-
chanical strength of the ceramic substrate. Previous studies
have shown ceramic cleaners, such as Ivoclean (Ivoclar Vi-
vadent, Schaan, Liechtenstein), lead to more effective cleaning
and stronger bond strengths compared to water rinsing or us-
ing phosphoric acid.5,6,10–14 The effectiveness of other ceramic
cleaners such as ZirClean (BISCO, Inc., Schaumburg, IL)
and Katana cleaner (Kuraray Noritake Dental Inc., Okayama,
Japan) remain largely unknown. According to their manufac-
turers, each cleaning solution works by a different mechanism
of action. Ivoclean is an alkaline cleaning solution composed
of hyper-saturated zirconia particles which attracts contami-
nants via a chemical gradient from the surface of the restora-
tion. This allows the contaminants to be rinsed away with wa-
ter before cementation. ZirClean cleaning gel is an alkaline
non-abrasive cleaner composed of potassium hydroxide which
breaks the ionic bond between the contaminant and restorative
surface. Katana cleaner is an acidic (pH 4.5) ceramic cleaner
composed of a 10-methacryloyloxdecal dihydrogen phosphate
(MDP) salt which is proposed to remove contaminants intra-
orally and/or extra-orally. The hydrophobic group of the MDP
salt bonds to the contaminant. The exposed hydrophilic phos-
phate group allows it to be rinsed away with water. Some pre-
vious studies have also reported that sodium hypochlorite can
effectively clean saliva from zirconia.4,14–16
Ceramic primers that contain MDP are used to treat the sur-
face prior to cementation to enhance the bond strength of zir-
conia to the resin cement. The phosphate group of the MDP
bonds with the surface of the zirconia, while the methacrylate
end bonds the resin cement. However, it has been suggested
to use MDP as a preventive measure against initial contami-
nation due to the phosphate group bonding the zirconia sur-
face, thereby exposing the hydrophobic methacrylate ends of
the monomer. The exposure of the hydrophobic ends creates
a boundary, preventing surface wetting by saliva. Angkasith et
al, concluded that if an MDP primer was used prior to try-in,
the surface may be cleaned with 20 seconds of water rinsing.10
This study aims to evaluate the bond strength of resin cement
to zirconia after cleaning the zirconia surface from saliva con-
tamination using different cleaning methods, and to determine
any significant differences in bond strength between zirconia
cleaning solutions. The null hypotheses are that there will be
no significant effect of cleaning method on the bond strength
between resin cement and zirconia, and there will be no differ-
ence in bond strength after the use of different cleaning solu-
tions.
Materials and methods
One-hundred and twenty square-shaped (10 mm × 10 mm ×
1.5 mm) zirconia samples (KATANA STML, Noritake Inc.,
Okayama, Japan) were fabricated for this study. Surface finish-
ing was performed using a series of silicon carbide grits (600
and 1200) at 300 rpm for 30 seconds each. Samples were then
sintered according to manufactures’ instruction and inspected
for any visible defects and then mounted in acrylic resin
(VariDur 200, Buehler, Lake Bluff, IL) for placement within
the shear bond fixture. Each sample was particle abraded with
2 Journal of Prosthodontics 00 (2021) 1–6 © 2021 by the American College of Prosthodontists
Sulaiman et al
50 µm aluminum oxide at 2.5 bar pressure (10 seconds) at
10 mm distance (Microetcher IIA, Danville Materials, San
Ramon, CA) and ultrasonically cleaned in distilled water for
2 minutes followed by drying with a stream of air. After sur-
face abrasion, samples were divided into 12 groups (n = 10)
(Fig 1 Table 1) for testing. The sample size was calculated
using G*Power v. 3.1.9.3 (Heinrich-Heine-Universität Düssel-
dorf, Germany). Input values were set as: Effect size f = 0.40,
α err prob = 0.05, Power (1-β err prob) = 0.80. The total sam-
ple size was determined to be 120 (n = 10/group) with an ac-
tual power = 0.8217.
In the control group (Group 1) a ceramic primer (Clearfil
Ceramic Primer Plus, Kuraray Noritake Dental Inc., Okayama,
Japan) was applied with agitation for 10 seconds using an ap-
plicator brush then dried for 5 seconds with a dry-air stream
prior to cement application. In Group 2, specimens were coated
with the ceramic primer for 10 seconds and dried, followed by
contamination with human saliva spread with a microbrush for
3 minutes. Saliva used in this study was collected from a single
participant and was stored in a sterile container at 4°C (up to 6
hours) until tested [Institutional Review Board (IRB#273921)].
Groups 3 to 12: saliva was applied to the zirconia surface and
spread with a microbrush for 3 minutes before rinsing with wa-
ter and drying, cleaned (different methods), then coated with
the ceramic primer. In Group 3, samples were cleaned (af-
ter contamination) with water rinsing only for 20 seconds. In
Group 4, samples were cleaned (after contamination) using the
initial abrasion protocol. Samples were treated with 4.5% hy-
drofluoric acid (HF, Group 5) or 35% phosphoric acid (Group
6) for 20 seconds and rinsed with water. Samples were cleaned
with Ivoclean (Group 7), Katana Cleaner (Group 8) or ZirClean
(Group 9) according to the application instructions of the man-
ufacturer. In Group 10, samples were cleaned with 4% sodium
hypochlorite for 20 seconds without agitation and rinsed. Sam-
ples were cleaned with 7.5% sodium hypochlorite with agita-
tion for 20 seconds (Group 11) and 60 seconds (Group 12) and
rinsed. Table 2 shows the composition, concentration, and pH
of the solutions used in the study.
Notched-edge shear bond strength test (NE-SBS, ISO ISO
29022) was used to evaluate bond strength to the zirconia
surface based on each cleaning method.17 Samples were cen-
tered and tightened in fixtures for bond strength testing (Ultra-
dent Products Inc., South Jordan, UT). Adhesive resin-cement
(Panavia V5, Kuraray Noritake Dental Inc., Okayama, Japan)
was inserted into an opening (Ø2.3 mm) in the plastic fixture.
The top-surface of the cement was polymerized for 10 sec-
onds using a polymerizing light (Elipar Deepcure-S, 3M, Saint
Paul, MN) with an average power of 960 mW. The samples
were stored in distilled water at 37°C for 24 hours and tested.
The NE-SBS test was performed using a Universal Instron ma-
chine (Model 4411, Instron, Norwood, MA). After a load cali-
bration, each sample was positioned horizontally in the testing
fixture and loaded at 1 mm/min until failure. The NE-SBS was
calculated from the peak failure load (MPa). The surface of
each sample was inspected under a stereomicroscope (100 ×),
and the failure type was recorded: adhesive, cohesive, or mixed
failure.
A one-way ANOVA was used to compare bond strength
values. The post-hoc tests for the pairwise differences were
Sulaiman et al
Grp1 Grp2
Grp3 Grp4
Grp5 Grp6
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
was considered statistically significant in two-tailed statistical
tests. All analyses were conducted using SPSS.
Results
The mean and standard deviation for each group is presented
in Table 1. A one-way ANOVA showed statistically significant
differences between the shear bond strength to zirconia follow-
ing different cleaning methods (Table 3, p < 0.001). Significant
differences between groups were determined with a Tukey post
hoc analysis (Table 1). The only cleaning method which did
not produce a lower bond strength than the control group in
which no contamination occurred was application of air-borne
particle abrasion following salivary contamination (p = 0.247).
There was no significant difference in bond strength between
the designated zirconia cleaning solutions (p = 0.105)
Discussion
The primary purpose of this study was to compare the effec-
tiveness of different cleaning methods after saliva contami-
Journal of Prosthodontics 00 (2021) 1–6 © 2021 by the American College of Prosthodontists
Cleaning Zirconia Bonding Surface
Grp 7 Grp 8
Grp 9
Grp 10
Grp 11 Grp 12
nation of a zirconia surface on shear bond strength of resin
cement to the surface. Achieving a long-lasting restoration is
dependent upon successfully creating a reliable bond between
the tooth structure and the restorative material. Failure to de-
contaminate a bonding surface is a frequent cause for bond
failure.18,19 Therefore, ensuring all bonding surfaces are free of
contaminants is important for the longevity of the restoration.
Try-in of zirconia restorations brings bonding surfaces into
contact with contaminants (saliva, blood, etc.) in the oral cav-
ity. Various techniques and cleaning methods exist for remov-
ing the organic contaminants and restoring the surface prior to
cementation.
Each test group was subjected to salivary contamination, fol-
lowed by the corresponding cleaning method and cementation.
The effectiveness of each cleaning method was determined
using NE-SBS. The results showed that there was a signifi-
cant difference in bond strength between the different meth-
ods, thus rejecting the null hypothesis. The uncontaminated
control group (Group 1) followed manufacturer recommended
instructions for surface preparation and cementation to the zir-
conia surface and hence it resulted in the highest bond strength
(25.3 MPa). The application of a ceramic primer prior to
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
inhibits the resin cement from bonding to the surface of the
zirconia,1,4,22 ultimately affecting the bond strength between
the resin cement and the zirconia surface which resulted in be-
ing the lowest amongst all cleaning methods (10 MPa).
Recently, the introduction of ceramic cleaners has provided
clinicians with a simple step-by-step cleaning method for
restoring ceramic surfaces after contamination. The manufac-
turer advertises Ivoclean as an alkaline extraoral universal ce-
ramic cleaner. Ivoclean has been reported as an effective way
of restoring ceramic surfaces.10,14 Ivoclean is a solution com-
posed of highly concentrated zirconia oxide particles which
form a concentration gradient, creating an increased affinity
for phosphate as compared to the ceramic surface. Increased
affinity in the solution removes organic contaminants from the
zirconia surface which can then be rinsed away with water. Zir-
Clean is also an alkaline cleaner for use on zirconia and other
ceramic restorations after try-in. Its alkalinity is due to potas-
sium hydroxide which interrupts the ionic bond formed be-
tween the contaminant and the zirconia surface.23 Unlike Ivo-
clean and ZirClean, Katana Cleaner is acidic (pH 4.5) which
allows either extraoral or intraoral application. The manufac-
turer advertises the product as a universal cleaner capable of
removing contamination from a wide variety of dental materi-
als and tooth structure. An MDP salt acts as the active ingredi-
ent, in which the hydrophobic methacrylate ends of the MDP
molecule attach to the organic contaminants which weakens
the bond to the restorative surface.24 The hydrophilic phos-
phate heads surround the contaminants, which allow them to
be washed away with water. Limited information regarding the
cleaning effectiveness of ZirClean and Katana Cleaner is avail-
able from previous invitro studies. Based on the results of the
present study, there was no significant difference in shear bond
strength between the ceramic cleaners, each effectively remov-
ing organic contamination and restoring the bonding surface.
Therefore, the second null hypothesis was accepted.
Sodium hypochlorite (NaOCl) was also considered as a
cleaner in this study due to its common use in dentistry as an
irrigant with strong antimicrobial properties. It has also been
shown that the effectiveness of NaOCl as a disinfectant is de-
pendent on its concentration.25 To investigate how varying con-
centrations of NaOCl would restore the surface of zirconia,
a 4% NaOCl, commonly used as an endodontic irrigant, and
household Clorox bleach (7.5% NaOCl) were used. Increas-
ing the concentration of NaOCl had no significant effect on the
shear bond strength. 7.5% NaOCl was also investigated un-
der different scrubbing times (20 and 60 seconds) to investi-
gate whether time of scrubbing may play a role in effectively
cleaning the surface and enhance the bond strength. Results in-
dicated that increased scrub time increased the bond strength
from 14.7 to 16 MPa. Further investigation is required to see
if NaOCl at higher concentration or longer scrubbing time can
effectively clean the surface. This can provide a more afford-
able alternative to zirconia cleaning solutions. It is important to
translate the outcomes from this study with care. This is an in
vitro study, and testing of the samples after a significant aging
period may be considered a more clinically relevant outcome
but was not considered in this study. The preliminary bond
strength after 24 hours was evaluated to determine the imme-
diate effect of each cleaning method on the bond strength, and
Journal of Prosthodontics 00 (2021) 1–6 © 2021 by the American College of Prosthodontists
Cleaning Zirconia Bonding Surface
any deterioration in bond strength due to aging may be consid-
ered as an expected outcome. The surface of each sample was
examined under 100 × magnification to identify the nature of
the failure as adhesive or cohesive. Adhesive failure was ob-
served unanimously in all groups, which was expected due to
the values reported of the bond strength of the resin cement to
the zirconia (Fig 1). No further magnification or analysis was
required.
Conclusion
There are different methods to clean the zirconia surface with
air-borne abrasion appearing to be the most effective, despite
its controversy. Designated zirconia cleaners and hydrofluo-
ric acid may decontaminate the zirconia surface promoting a
stronger bond of the resin cement to the zirconia.
Conflict of interest statement
The authors deny any conflicts of interest in regard to this
study.
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