ORIGINAL RESEARCH

Effect of Various Surface Treatments of Zirconia on its

A b s t r ac t
Aim: To assess the effectiveness of various surface treatments and adhesives on the bond strength of zirconia-based ceramic to dentin.
Materials and methods: Eighty samples of zirconia were subjected to the four-surface treatment protocols (sandblasting, 48% hydrofluoric acid
(HF), 48% hydrofluoric acid + 70% nitric acid (HNO3) and no treatment (control) following which the samples from each group were subdivided
into two subgroups (n = 10) based on the resin cement employed for cementation (RelyX U200 and G-Cem Linkforce). The bonded specimens
were subjected to shear stress to measure the bond strength using Universal testing machine. To test the difference in bond strength among
the eight study groups, the Kruskal–Wallis ANOVA test was applied and for comparison between cements in each group, Mann–Whitney U
test was applied.
Results: The highest bond strength values were observed for 48% HF group cemented with G-Cem Linkforce resin cement (16.220 ± 1.574)
and lowest for control group–RelyX (4.954 ± 0.972). G-Cem cement showed higher bond strength than RelyX for all surface treatments except
48% HF + 70% nitric acid.
Conclusion: It can be inferred that 48% HF can etch zirconia and generate a porous structure that proves to be beneficial for bonding.
Clinical significance: The increasing demand for esthetics has led to the replacement of metal-ceramic materials with zirconia-based ceramics.
However, the chemical inertness of zirconia to various conventional surface treating agents has continuously challenged researchers to discover
a new surface treatment protocol that could enhance the bond strength of zirconia.
Keywords: Bond strength, Resin cements, Sandblasting, Zirconia.
The Journal of Contemporary Dental Practice (2024): 10.5005/jp-journals-10024-3663

Introduction 1–3,5,6
Department of Conservative Dentistry and Endodontics, Amrita
The increasing requirement for esthetics has guided dental School of Dentistry, Amrita Vishwa Vidyapeetham, Kochi, Kerala, India
professionals to prefer all-ceramic materials over metal and 4
Department of Public Health Dentistry, Amrita School of Dentistry,
porcelain-fused metal-ceramic restorations for oral rehabilitation Amrita Vishwa Vidyapeetham, Kochi, Kerala, India
which can be attributed to its advantageous optical properties Corresponding Author: Asha Joseph, Department of Conservative
like translucency, biocompatibility, low thermal conductivity as Dentistry and Endodontics, Amrita School of Dentistry, Amrita Vishwa
well as low wear resistance, and low abrasiveness.1 However, the Vidyapeetham, Kochi, Kerala, India, Phone: +91 9746473521, e-mail:
applications of all-ceramic restorations are limited due to their ashjohan81@[Link]
brittleness, sensitivity to flaws and defects, low tensile strength, How to cite this article: Yenamandra MS, Joseph A, Singh P, et al. Effect
and fracture toughness.2 Recently, high-strength zirconia ceramics of Various Surface Treatments of Zirconia on its Adhesive Properties to
have become a highly recommended material in dentistry because Dentin: An In Vitro Study. J Contemp Dent Pract 2024;25(3):226–230.
of their favorable characteristics such as high flexural strength Source of support: Nil
and toughness, esthetics, and biocompatibility. 3 But adhesion to Conflict of interest: None
the tooth structure poses a challenge to every clinician as it is a
polycrystalline material that is resistant to conventional etching
techniques due to its silica-free structure.4 Many chemical and Several studies have reported conflicting results on the increase
mechanical pretreatment methods for zirconia surfaces have been and decrease in bond strength after sandblasting.
researched including sandblasting, hydrofluoric acid (HF) etching, Acid etching enables the homogenous roughening of
the use of a combination of hydrofluoric acid and nitric acid (HNO3) material regardless of its size and shape. Recently, various studies
tribochemical silica coating. However, an optimal resin bonding investigating the effectiveness of HF were found to be beneficial
technique for zirconia has not been established yet. Air abrasion for treating the zirconia surface and thus improving the resin-to-
with alumina particles often known as sandblasting, roughens the zirconia adhesion. 5–7 As demonstrated by Yen et al.,6 HF reacts
zirconia surface and aids in resin/ceramic micromechanical interlock preferentially with the silica phase in a glassy matrix to form
formation thereby increasing the bond strength. However, since the hexafluorosilicates rendering the surface of the ceramic rough.
microporosities created by sandblasting may act as crack-initiators Concentrations ranging between 4 and 10% HF acid are commonly
thereby weakening the ceramic restoration, it is imperative to used in a dental laboratory. However, various studies have proved
explore new methodologies that may enhance the long-term that higher concentrations of etchant can modify the surface
results and do not interfere with the properties of ceramics. 5 morphology of zirconia by creating a highly uneven surface.7

© The Author(s). 2024 Open Access. This article is distributed under the terms of the Creative Commons Attribution 4.0 International License ([Link]
org/licenses/by-nc/4.0/), which permits unrestricted use, distribution, and non-commercial reproduction in any medium, provided you give appropriate credit to
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 Effect of Various Surface Treatments on Zirconia

Treatment with 48% HF for a shorter period proved to be effective Flowchart 1: Flowchart for different groups with subgroups
in creating deep micro-retentions on the topographic surface of
zirconia in a more uniform manner when compared to that with
sandblasting.5 Recently, a mixed solution of HF and nitric acid has
been introduced that was shown to create surface irregularities
on the zirconia samples which were more uniform and detailed
than those treated with sandblasting alone.8 Only a few studies
have noted the combination HNO3/HF etching and it has shown
that this combination significantly roughens the zirconia surface.
Cement selection is also an important prerequisite as the quality
and longevity of its bond strength to zirconia ceramic profoundly
determines the clinical success of the restoration. Resin cements
can be classified as conventional resin cement and self-adhesive
resin cement based on the bonding mechanism. Self-adhesive
resin cements belong to a new category of resin cements that along
with the ease of application, offer a few advantages of adhesive
resin cements such as increased compressive strength and shear
bond strength together with a good marginal seal.9 These cements
do not require technique-sensitive steps like etching, priming or
bonding. G-Cem is a dual-cure adhesive resin cement, containing
methacryloyloxydecyl dihydrogen phosphate (MDP) which shows
excellent bonding to zirconia due to its chemical interaction between
the functional phosphoric acid monomer and the hydroxyl groups of
the passive zirconia surface. RelyX U200 is yet another dual cure self-
etch resin cement which in addition to conventional methacrylate
monomers contains methacrylate monomers with phosphoric acid
groups as well as unsaturated carbon-carbon double bonds.
Luting zirconia is highly challenging as most surface treatments • Group I (G I): No surface treatment–control group.
do not result in significant alteration of the surface due to the high • Group II (G II): Sandblasting was carried out with 50 µm aluminum
crystalline content and limited vitreous phase of this ceramic. oxide particles for 10 seconds at 2 bar pressure and at a distance
Though zirconia restorations can be luted using conventional of 10 mm.10,11
cements, the choice of resin luting cements offers reliable bonds • Group III (G III): The samples were etched with 48% HF solution
with higher bond strength. However further research targeting the (NICE chemicals Pvt. Ltd, Kerala, India) with a micro applicator
adhesiveness of MDP-based resin cements to zirconia along with tip for 2 minutes and rinsed with deionized water for 1 minute
different zirconia surface pretreatment methods is necessary for and then gently air-dried. 5
product evaluation. • Group IV (G IV): The samples were etched with 48% HF + 70%
The objective of this study was to assess the effectiveness of HNO3 solution with a micro applicator tip for 2 minutes and were
various surface treatments along with different resin cements on rinsed thoroughly with distilled water (NICE chemicals Pvt. Ltd,
the bond strength of zirconia-based ceramic to dentin. Kerala, India) and dried.5
The samples in each group were further subdivided into two
M at e r ia l s and Methods subgroups with ten samples each based on the resin cement used
In the present in vitro study, 80 caries-free sound permanent for luting (Flowchart 1):
maxillary and mandibular premolars extracted for orthodontic • A: RelyX U200 (3M, Germany): The cement was dispensed and
purposes were selected. mixed for 20 seconds and applied on the treated zirconia surface.
Tooth Preparation The zirconia sample was cemented onto the exposed dentin
surface. The cement was then light-cured on each side for 20
The occlusal surface of the selected teeth was prepared to create a
seconds according to the manufacturer’s recommendations.
uniform dentinal surface. The prepared teeth were then embedded
• B: G-Cem Linkforce (GC corporation, Tokyo): Total etch technique
in an autopolymerizing resin such that the exposed dentinal surface
was adopted for surface treatment of tooth structure followed
was available for the cementation of zirconia samples until the
by application of the bonding agent (G-Premio bond, GC
bonding procedure.
America Inc.) for 10 seconds, air dried for 5 seconds, and light
Sample Preparation and Surface Treatment cured for 10 seconds based on manufacturer’s instructions. The
zirconia samples were coated with the primer (G-Multi Primer,
A prototype of the Zirconia disc (Ceramill Zolid HT+, Denspro,
GC America Inc.) and dried. The cement was injected onto the
Germany) was fabricated using a CAD/CAM system, measuring
cementing surface of zirconia which was seated over the treated
3 mm in height and 4 mm in diameter. Using this prototype, 80
tooth surface and light cured.
cylindrical samples of zirconia were milled from 4 blanks and were
allotted into 4 main groups randomly (n = 20) based on surface Following the bonding procedure, specimens were stored in
treatment protocol (Flowchart 1). distilled water at room temperature until testing within 24 hours.

The Journal of Contemporary Dental Practice, Volume 25 Issue 3 (March 2024) 227
 Effect of Various Surface Treatments on Zirconia

Table 1: Mean ± SD of shear bond strength values of different study Table 2: Comparison of median shear bond strength between the
groups study groups
Group (n = 10) Mean ± SD (MPa) Group (n = 10) Median IQR p-value Order
Control–RelyX (GIA) 4.954 ± 0.972 Control–RelyX 5.083 4.325–5.746 <0.001* 8
Control G-Cem (GIB) 6.752 ± 0.740 (GIA)
Sandblasting RelyX (GIIA) 8.629 ± 0.850 Control–G-Cem 6.792 6.051–7.482 7
(GIB)
Sandblasting G-Cem (GIIB) 12.996 ± 0.821
Sandblasting– 8.941 7.812–9.335 <0.001* 6
48% HF RelyX (GIIIA) 14.027 ± 0.845 RelyX (GIIA)
48% HF G-Cem (GIIIB) 16.220 ± 1.574 Sandblasting– 12.790 12.340–13.710 3
48% HF + 70% HNO3 –RelyX (GIVA) 12.389 ± 0.744 G–Cem (GIIB)
48% HF + 70% HNO3 –G-Cem (GIVB) 11.281 ± 0.773 48% HF–RelyX 13.857 13.511–14.556   0.002* 2
(GIIIA)
48% HF–G-Cem 15.708 15.095–17.798 1
Assessment of Shear Bond Strength (SBS) (GIIIB)
The samples were mounted onto a custom-made jig and subjected 48% HF + 70% 12.308 11.940–12.804   0.003* 4
to shear stress using a Universal testing machine at a crosshead HNO3 –RelyX (GIVA)
speed of 0.5 mm/minute until the debonding occurred. The force
48% HF + 70% 11.453 10.774–11.877 5
at which the samples de-bonded was expressed in Newtons (N).
HNO3 –G-Cem
The resultant SBS was obtained in megapascals (MPa) by dividing (GIVB)
the maximum force obtained in Newton by the cross-sectional area
p-value < 0.001*
(mm2) of the bonding surface for each specimen.
The formula used for the calculation was as follows:
• Area of the bonded surface (mm2) = π × r2 (r–radius in mm).
• Shear bond strength (MPa) = Force (N)/Area of bonded surface
(mm2).

Statistical Analysis
Observed data was coded, tabulated, and analyzed using SPSS
Version 20 for Windows. Shear bond strength was calculated
according to the prescribed formula and expressed as mean
and standard deviation. Since the data did not follow normal
distribution, the values were represented as median and
interquartile range and to test the statistical significance of the
difference in bond strength among the four groups, Kruskal–Wallis
ANOVA was applied. To compare the bond strength between two
resin cements in each of the surface treatment groups, the Mann–
Whitney U test was applied.
A p-value of less than 0.05 was considered statistically
significant.

R e s u lts Fig. 1: Box plot-depiction of the shear bond strength values among the
groups through their quartiles
A total of 80 samples (10 in each group) were analyzed. Table 1
shows the mean and standard deviation of shear bond strength of
the study groups. The highest shear bond strength was noted for
the group that used surface treatment—48% HF luted with G-Cem 48% HF–RelyX (GIIIA) (13.85, IQR: 13.51–14.55), sandblasting-G-Cem
resin cement (16.220 ± 1.574) and the least for control–RelyX (4.954 ± (GIIB) (12.79, IQR: 12.34–13.71), 48% HF + 70% HNO3–RelyX (GIVA)
0.972). Luting with G-Cem showed higher mean bond strength for (12.30, IQR: 11.94–12.80), 48% HF + 70% HNO3–G-Cem (GIVB) (11.45,
all surface treatments except for 48% HF + 70% HNO3. IQR: 10.77–11.87), sandblasting-RelyX (GIIA) (8.94, IQR: 7.81–9.33),
The null hypothesis was that the surface treatments of zirconia, control–G-cem (GIB) (6.79, IQR: 6.05–7.48) and control-RelyX (GIA)
with either sandblasting or acid etchants, followed by cementation (5.08, IQR: 4.32–5.74).
with either self-adhesive resin or MDP containing self-etch resin, A subgroup analysis was done based on the cement used for
would not affect the bond strength of the zirconia to tooth structure luting (Table 3). Thus, the highest bond strength was noted for 48%
when compared to the control group. HF with G-Cem and the least for the Control group RelyX.
A comparison of median and IQR values between 8 groups
revealed a statistically significant difference (p < 0.001) (Table 2 Discussion
and Fig. 1). The highest mean SBS values were seen in 48% HF and In the recent decade, zirconia-based ceramics have gradually gained
cemented with G-Cem cement (15.70 IQR: 15.09–15.79) followed by popularity as a promising biomaterial owing to the escalating

228 The Journal of Contemporary Dental Practice, Volume 25 Issue 3 (March 2024)
 Effect of Various Surface Treatments on Zirconia

Table 3: Comparison of median shear bond strength between the group would have also contributed to better bond strength values
subgroups (Resin cements) as functional monomers like MDP assure adhesion to enamel
Resin cement Surface treatment Median (IQR) p-value and dentin tissues, since the phosphoric acid and carboxylic acid
functional groups of those monomers can chemically bond to
RelyX Control 5.08 (4.32–5.74) <0.001
calcium.
Sandblasting 8.94 (7.81–9.33) In the current study, G-Cem Linkforce showed higher bond
48% HF 13.86 (13.51–14.55) strength values than the RelyX U200 resin cement which can
48% HF + 70% HNO3 12.31 (11.94–12.80) be explained by its excellent hydrolytic stability owing to the
G-Cem Control 6.79 (6.04–7.48) <0.001 presence of a functional monomer (MDP).17 G-Multi Primer that
was coated onto the zirconia surface before the application of
Sandblasting 12.79 (12.34–13.70)
G-Cem Linkforce resin cement, incorporates three main functional
48% HF 15.71 (15.09–17.79) agents (silane, phosphate, and thiophosphate monomers), which
48% HF + 70% HNO3 11.45 (10.77–11.88) provide adhesion to various substrates. The objective of adding
silane to the primer is to enhance the stability of the bond.6 The
MDP monomers stimulate the formation of a chemical bond to
demand for esthetics. However, the inertness of zirconia to the oxide group of zirconia via two hydrogen groups derived
traditional chemical and mechanical surface treatment methods from the phosphate group forming a Zr-O-P covalent bond.18,19
that are applicable to glassy ceramics has compelled the researchers This Zr-O bond formation was confirmed by Byeon et al. proving
to explore an alternative strategy.12 the establishment of a chemical bond between zirconia and MDP
Various studies have been carried out using several other strong monomer.20
acids such as nitric acid, sulfuric acid, and hydrochloric acid.13 In However, the bond strength values of 48% HF + 70% HNO3
the present study, the effects of sandblasting, HF etching alone treated samples cemented with G-Cem Linkforce luting agent
and a combination of HNO3/HF-etching on the zirconia surface (GIVB) were found to be less than that of those cemented with
were investigated by examining the shear bond strength between RelyX U200 cement (GIVA) probably because this self-adhesive
zirconia and adhesive resin cement. The current study employed resin cement percolates through spaces in the roughened surface
the use of the G-Cem Linkforce system and RelyX U200 to maximize to form microchemical interlocks and the inorganic filler in the
the bonding effectiveness of the zirconia. cement is more resistant to hydrolytic degradation.8 This finding is
Extracted natural teeth were used in the current study as in concurrence with the results obtained by Oyagüe et al.21
they exhibit properties such as modulus of elasticity, thermal The samples belonging to sandblasting surface treatment
characteristics, strength and bonding features that are closer to the group displayed better bond strength values than that of the control
clinical scenario. Zirconia samples were milled using a prototype group which could be because sandblasting with alumina particles
fabricated from CAD/CAM as this technology standardizes the generates a rough surface accompanied by a greater surface energy
design and fabrication of samples thereby delivering identical and wettability thereby enhancing the resin to zirconia bond The
specimens for the in vitro studies of restoration materials, cements, tetragonal-monoclinic (t-m) phase transformation generated
or bonding techniques.14 by sandblasting of zirconia induces compressive stresses on the
The SBS values upon applying 48% HF solution were found to surface which counteracts the deleterious effects associated with
be more than that of the control group as it caused the dissolution it. However, the further progression of this phase transformation
of surface zirconia particles.8 Furthermore, the SBS values of the may develop tensile residual stresses thereby decreasing the
mixed etching solution were merely more than the sandblasting flexural strength of the material. The effect of sandblasting on the
group but less than that of the 48% HF group indicating reduced flexural strength of zirconia is disputable with regard to the power
surface roughness created by the combined acid etching solution. and duration of the procedure. 22 In the present study, wherein
Similarly, Liu et al. found that the surface roughness created by the sandblasting group that was cemented with resin cement
the combination of HF and HNO3 acid solution was only 21% of containing MDP monomer (G-Cem Linkforce) gave higher SBS
that created by the HF acid.15 Similar findings were also observed values than the ones cemented with resin cement without the
in a study by Goyata et al. wherein, a combination nitric acid and monomer (RelyX U200).23
HF solution proved to be less effective in increasing the surface
roughness of zirconia when compared to that of 48% HF alone.5
The samples etched with HF alone and luted using G-Cem Linkforce C o n c lu s i o n
exhibited the highest bond strength probably due to the presence Surface treatments based on HF etching, HF and HNO3 combination
of Zr-F bonds on HF-treated zirconia which improves the surface significantly increased the bond strength of Zirconia compared
reactivity and due to the formation of fine and uniform nano- to that observed in untreated specimens. The MDP molecule
scale pits along with enlarged surface area when the zirconia was containing resin cement (G-Cem) showed better bond strength
pretreated with HF. Such a shallow surface architecture advocates compared to self-adhesive resin cement. Further studies on
increased adhesion without forming deep and excessive surface strategies to enhance the adhesive strength of zirconia such as
damage that can weaken the treated zirconia. Quentin et al. alteration in duration, concentration and temperature of the etchant
demonstrated that a higher concentration of HF was required to are necessary. Additional in vivo trials will be needed to authenticate
etch the zirconia surface at room temperature, as it created an these in vitro results. Also, the effects of aging on Zirconia-resin
accelerated and highly uniform etch pattern.16 The use of MDP- bonding to mimic a clinical setting using these pre-treatment
containing adhesive resin cement along with this HF pretreatment methods should be evaluated in further studies.

The Journal of Contemporary Dental Practice, Volume 25 Issue 3 (March 2024) 229
 Effect of Various Surface Treatments on Zirconia

Ethical Approval different dental zirconia grades. Materials (Basel) 2021;14(3):610. DOI:
10.3390/ma14030610.
The review was approved by the Institutional Ethics Committee
11. Harb O, Al-Zordk W, Özcan M, et al. Influence of hydrofluoric and
of Amrita Institute of Medical Sciences (IRB-AIMS-2019-161 dated nitric acid pre-treatment and type of adhesive cement on retention
19-03-2019). of zirconia crowns. Materials (Basel) 2021;14(4):960. DOI: 10.3390/
ma14040960.
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