RESEARCH AND EDUCATION

Evaluation of the bond strength and characteristics of zirconia

after different surface treatments
Virgílio Vilas Boas Fernandes Júnior, DDS, MS,a Débora Cristina Barbosa Dantas, DDS, MS,b
Eduardo Bresciani, DDS, PhD,c and Maria Filomena Rocha Lima Huhtala, DDS, PhDd

Zirconia is a biocompatible ABSTRACT

and bioinert ceramic with Statement of problem. Non-thermal plasma treatment could increase the bond strength of resin
high mechanical strength, cements to zirconia, but studies are lacking.
chemical stability, low thermal
Purpose. The purpose of this in vitro study was to evaluate zirconia bond strength, surface
conductivity, and excellent es-
roughness, and contact angle and to measure the infrared spectrum after different surface
thetics.1-4 These properties treatments.
have led to its increased
popularity for dental prosthe- Material and methods. Yttria-tetragonal zirconia polycrystal (Y-TZP; n=9) blocks were sectioned
into 36 slices (12×11×3 mm) and divided (n=4) into surface treatment groups as follows: 2 control
ses. However, zirconia has a
groups, consisting of airborne-particle abrasion plus primer (APP) and 10% hydrofluoric acid etching
low surface energy, which re- plus primer (HFP), and 3 experimental groups consisting of a nonthermal plasma (NP) application; a
stricts adhesiveness after nonthermal plasma plus primer application (NPP); and a 10% hydrofluoric acid etching plus
cementation, even with resin nonthermal plasma plus primer (HFNPP) application. Each zirconia disk was cemented to a
cements and surface treat- prepolymerized resin block. After cementation, the specimens were sectioned for microtensile
ments with acid or airborne- strength testing and for surface roughness analysis and contact angle analysis. Results were
particle abrasion followed by submitted to analysis of variance and Tukey tests (a=.05).
5-8
primer application. Unlike Results. Results showed no statistically significant differences between the APP and HFNPP groups,
other dental ceramic materials, but these 2 groups showed statistically better bonding than those of HFP, NP, and NPP.
zirconia has a polycrystalline Conclusions. Airborne-particle abrasion resulted in a significant increase in surface roughness
composition without a glassy compared with the other groups. After nonthermal plasma treatment, the contact angle of the
phase, thus allowing high zirconia surface decreased within 48 hours. Nonthermal plasma application for surface treatment of
chemical stability and better zirconia showed no significant difference in bond strength when compared with airborne-particle
resistance to acid corrosion.9 abrasion. (J Prosthet Dent 2018;-:---)
Until now, airborne-particle
abrasion with silica-coated aluminum oxide particles has airborne-particle abrasion is associated with micro-
been the best way to create micromechanical retention in cracking of the zirconia, which may impair long-term
zirconia restorations. The abrasive action changes the restoration performance.13-15
surface with the incorporation of silica-coated aluminum Nonthermal plasma application is a surface treat-
particles. This creates a more reactive surface for silani- ment that has been used for polycrystalline materials.
zation and also better interaction with the resin An interaction between the plasma ions and electrons
cement.10-12 However, the improved retention after breaks down stabilized radicals, thus promoting

a
Doctoral student, Graduate Implantology, Department of Restorative Dentistry, Institute of Science and Technology, São Paulo State University,
São José dos Campos, Brazil.
b
Doctoral student, Department of Restorative Dentistry, Institute of Science and Technology, São Paulo State University, São José dos Campos, Brazil.
c
Associate Professor, Department of Restorative Dentistry, Institute of Science and Technology, São Paulo State University, São José dos Campos, Brazil.
d
Associate Professor, Department of Restorative Dentistry, Institute of Science and Technology, São Paulo State University, São José dos Campos, Brazil.

THE JOURNAL OF PROSTHETIC DENTISTRY 1

2 Volume
Clinical Implications
Nonthermal plasma surface treatment for zirconia
does not cause structural damage and promotes
effective adhesion. Such treatment may be an
essential factor for the longevity of zirconia
prostheses.
decontamination and increasing surface reactivity.16-20
Plasma is described as the fourth state of matter in
addition to the solid, liquid, and gaseous states. Plasma
is used in the manufacture of monitors and fluorescent
lamps, the treatment of solid surfaces, and more
recently in the biomedical sector.21-22 Different sources
of atmospheric plasma are available for applications.23
In dentistry, if correctly and efficiently used, dentin
plasma treatment removes contamination and prepares
the dentin for strong and durable adhesion to restor-
ative materials.24-27
The objective of this study was to assess the bond
strength, surface roughness, and contact angle and to
measure the infrared spectrum of yttria-tetragonal zirconia
polycrystal (Y-TZP) after conventional and experimental
surface treatments with nonthermal argon plasma. The
null hypothesis was that treating the surface of the Y-TZP
with nonthermal plasma before cementation would not
influence the bond strength, would not influence surface
roughness, and would not influence the contact angle.
MATERIAL AND METHODS
Ten Y-TZP blocks were sectioned into 4 specimens each
(14.5×15.5×4 mm); these specimens were sintered and cut
into slices (12×11×3 mm). The slices were polished by
using 600- and 800-grit silicon carbide paper disks
mounted on a polishing machine (Labcut 1010; Extec
Corp) under water irrigation. The surface of the slices was
submitted to different treatments before cementation and
bond strength testing, surface roughness and contact angle
analyses, and surface infrared spectroscopy measurement.
For microtensile strength testing, specimens were
divided into 5 groups: 2 control groups and 3 experi-
mental groups. The 2 control consisted of an airborne
particle abrasion with silica-coated aluminum oxide
particles (Rocatec Plus; 3M ESPE) plus primer (Mono-
bond Plus; Ivoclar Vivadent AG) (APP) application, and
a 10% hydrofluoric acid application plus primer (HFP)
group. The hydrofluoric acid was applied to specimens
for 1 minute, washed with air-water spray for 1 minute,
cleaned with 37% phosphoric acid (Condac; FGM
Produtos Odontológicos) for 1 minute, washed with
air-water spray for 30 seconds, and then dried with an
THE JOURNAL OF PROSTHETIC DENTISTRY
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air jet for 1 minute before application of the primer.
The 3 experimental groups consisted of a nonthermal
argon plasma (NP) application throughout the surface
for 1 minute at 10 mm; a plasma plus primer (NPP)
application; and a hydrofluoric acid plus plasma plus
primer (HFNPP) application. Specimens were cemen-
ted onto previously made resin blocks (Filtek Z350 XT;
3M ESPE) by using resin cement (Multilink N; Ivoclar
Vivadent AG). The materials used are described in
Table 1.
A surface plasma treatment device (model SAP; Sur-
face - Engenharia e Soluções a Plasma Ltd) was used at
room temperature (22 C) for nonthermal plasma appli-
cation. Argon gas (Praxair 4.8; White Martins Gases Ind
S.A.) was used at a mass flow rate of 1 l/min, generating a
plasma flow of 20 mm in length. The cannula’s tip was
positioned at 10 mm from the surface to be treated, and
the exposure time was 1 minute. Plasma was vertically
applied to the surface during application, with the flow
covering the area to be treated.
Composite resin blocks had been previously pre-
pared in a silicone matrix of the same dimensions as
the zirconia slices. On the matrix, 2-mm increments of
composite resin (A3, Filtek Z350 XT; 3M ESPE) were
inserted and light-polymerized for 20 seconds by using
a light-emitting diode device (Radii-cal; SDI Ltd) at an
irradiation of 1200 mW/cm2. The resin blocks were
cemented to the zirconia slices after the surface treat-
ments, using an autopolymerizing resin cement (Mul-
tilink N; Ivoclar Vivadent AG). The cement was applied
to the entire surface of the slice before the placement of
the resin block. The blocks of composite resin were
held in a position coincident with the zirconia slice
surface. Excess cement was removed, and the specimen
remained for 8 minutes until complete polymerization.
After 48 hours’ storage, the specimens were mounted
in a chemically activated acrylic resin base with wax,
positioned on the cutting machine (Labcut 1010; Extec
Corp), and sectioned perpendicularly to the adhesive
joint producing resin zirconia microtensile specimens
of approximately 1 mm in thickness (36 to 48 per
group). Specimens were stored in deionized water at
37 C for 24 hours before microtensile bond strength
testing. Each specimen was measured with digital cal-
ipers before being tested in a universal testing machine
(DL-200MF; EMIC) at a cross-head speed of 1 mm/min
and a 100-N load cell, according to International Or-
ganization for Standardization (ISO) TS 11405. At
failure, the test was automatically stopped and the data
recorded.
For surface roughness, 4 slices were used, which were
divided into 4 groups as follows: no surface treatment
(NT), 10% hydrofluoric acid (HF), nonthermal plasma
Vilas Boas Fernandes Júnior et al
- 2018 3

Table 1. Description of materials used Table 2. Characteristics of zirconia after surface

Material Composition Manufacturer treatment (mean ±SD)
Multilink N Dimethacrylate, HEMA, and Ivoclar Vivadent AG Treatment Bond Strength (MPa)*
inorganic particles HFP 8.88 ±5.15A
Monobond Plus Alcohol, sulfide dimethacrylate, Ivoclar Vivadent AG APP 11.69 ±5.97AB
MDP, gamma-MPTS
HFNPP 13.26 ±5.75B
Filtek Z350 XT BisGMA, BisEMA, UDMA, TEGDMA, 3M ESPE
nanoparticles of zirconia/silica
Treatment Surface Roughness (mm)*
Porcelain conditioner 10% hydrofluoric acid Dentsply Sirona
NT 0.094 ±0.008A
Condac 37% phosphoric acid FGM Produtos
Odontologicos HF 0.137 ±0.015B
NP 0.152 ±0.028B
Bis-EMA, bisphenol A diglycidyl methacrylate ethoxylated; Bis-GMA, bisphenol A digly-
cidyl methacrylate; gamma-MPTS, gamma-methacryloxypropyltrimethoxysilane; HEMA, APA 0.264 ±0.009C
hydroxyethyl methacrylate; MDP, 10-methacryloxydecyl dihydrogen phosphate; TEGDMA:
triethylene glycol dimethacrylate; UDMA, urethane dimethacrylate. Treatment Contact Angle (degrees)*
NT 74.65 ±10.84A
HF 49.04 ±7.68B
application (NP), and airborne-particle abrasion (APA). NP 45.56 ±15.65B
Specimens were analyzed by a white light interferometry APA 47.94 ±10.73B
(Zygo NewView 200; Artisan Technology Group). Five APP, airborne-particle abrasion plus primer; HFNPP, 10%
measurements of different regions of each specimen hydrofluoric acid etching plus nonthermal plasma plus
primer application; HFP, 10% hydrofluoric acid etching
were recorded. plus primer. *Different superscript letters mean signifi-
For measurement of the contact angle, 20 zirconia cant differences in bond strength of zirconia among
treatment groups (P<.05).
slices were used, which were divided into the same
treatment groups as for surface roughness (NT, HF, NP,
and APA). One specimen from each group was analyzed Cohesive in resin Mixed Adhesive
immediately after surface treatment, another after 12
100%
hours, and another after 24 hours. A drop of deionized
water (approximately 10 mL) was dripped onto the 90%
treated surface of zirconia slice from each group at room 80%
temperature. The contact angle was measured with a 70%
goniometer (TL100 Attension; Biolin Scientific) and data
Failure (%)

60%
recorded at 12 frames per second during 15 seconds after
the drop touched the surface. This process was repeated 50%
3 times on each specimen. Excess water between drops 40%
was removed with absorbent paper. 30%
A Fourier transform infrared spectrometer (FTIR;
20%
Frontier; Perkin Elmer), was used to characterize the
10%
chemical bonds at the zirconia surface. Three slices were
divided according to the following treatments: NT, APA, 0%
HFP APP HFNPP NP NPP
and 10% hydrofluoric acid plus nonthermal plasma
Group
(HFP). Specimens were assessed with a spectrometer
operating in the region of 400 to 500 cm−1 at a resolution Figure 1. Mode of failures for each group (%). APP, airborne-particle
of 4 cm−1 and 30 gains. abrasion plus primer; HFNPP, 10% hydrofluoric acid etching plus
nonthermal plasma plus primer; HFP, 10% hydrofluoric acid etching plus
The data generated were analyzed statistically by
primer; NP, nonthermal plasma; NPP, nonthermal plasma plus primer.
using software (Electronic Statistics Textbook 2013,
Statsoft Inc) with ANOVA and Tukey honest significant
group. Results of the 2-way ANOVA and Tukey HSD tests
differences (HSD) tests (a=.05).
for interactions for contact angle between the factors sur-
face treatment × time (immediately, after 12 hours, and
RESULTS
after 24 hours are listed in Tables 3, 4.
Groups P and NPP were excluded from bond strength Results of FTIR are presented in Figure 2. The spectral
analysis because they failed adhesively when the cemented curve patterns were similar between specimens subjected
blocks were cut into slabs. Table 2 lists the Tukey HSD test APA and those subjected to HFNP, and when compared
results for groups with different zirconia surface treatments with the NT group. This strongly suggests the presence
and Figure 1 shows the mode of failure percentages in each of −OH and −COOH radicals.

Vilas Boas Fernandes Júnior et al THE JOURNAL OF PROSTHETIC DENTISTRY

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Table 3. Two-way ANOVA Table 4. Interaction between surface treatment and

Effect SS df MS F P time on contact angle
Intercept 106156.5 1 106156.5 1244.439 <.001 Treatment/Time Mean ±SD (degrees)
Treatment 5026.7 3 1675.6 19.642 <.001 NT
Time 77.7 2 38.8 .455 .639 Immediate 84.55 ±5.06C
Treatment×Time 2168.7 6 361.4 4.237 .004 12 h 69.30 ±12.75AC

ANOVA, analysis of variance.

24 h 70.11 ±7.83AC
HF
Immediate 48.22 ±2.86AB
0.28 12 h 53.97 ±12.33AB
A (Absorbance percentage x100%)

0.26
24 h 44.94 ±3.60AB
0.24 APA
0.22 NP
0.20 Immediate 30.77 ±3.23B
HF+Plasma
0.18 12 h 43.24 ±2.46AB
0.16 24 h 62.68 ±13.70AC
0.14 Control
APA
0.12
0.10 Immediate 52.96 ±18.32AB
0.08 12 h 43.87 ±1.48AB
0.06 24 h 47.00 ±7.68AB
0.04
APA, airborne-particle abrasion; HF, 10% hydrofluoric acid; NP,
0.02
nonthermal plasma application; NT, no surface treatment; SD,
0.00 standard deviation. Different superscript letters mean significant
4000 3500 3000 2500 2000 1500 1000 550 differences in the interaction between surface treatment and time
Wave number cm–1 on contact angle (P<.05).

Figure 2. Fourier transform infrared spectrometer analysis. Similar

absorbance peaks for zirconia surface after sandblasting and after electrons with the micro-atmosphere around the exposed
hydrofluoric plus plasma application. APA, airborne-particle abrasion; area break down the stabilized weak bonds among them,
HF, 10% hydrofluoric acid.
thus promoting the formation of polar groups for new
chemical bonds.16,24 Plasma treatment destabilizes the
DISCUSSION
surface, making it reactive due to the formation of active
The first stated null hypothesis, that treating the surface radicals, mainly of oxygen and nitrogen.16,18 Another
of Y-TZP with nonthermal plasma before cementation explanation for the improved adhesion is the surface
would not influence the bond strength, was rejected. cleaning promoted by plasma through reduction of the
The second stated hypothesis, that nonthermal plasma number of hydrocarbons adsorbed during the breaking
would not influence zirconia surface roughness, was down of C-H and C-C radicals. Differently, from abra-
accepted, and the third hypothesis, stating that there sion and tribochemical treatment, plasma application
would be no change in the surface contact angle, was does not contaminate with impurities or modify the
also rejected. zirconia surface. This may affect the bond strength of
Zirconia has a low surface energy, limiting adhe- zirconia and its long-term stability.17
siveness following cementation, even when resin ce- This surface modification process, where polar groups
ments are used, and the surface has been treated with are created, caused the zirconia surface to become more
acid or airborne-particle abrasion plus primer applica- reactive and favor wettability, with consequent decrease
tion.5,6 It has virtually no glassy phase, which allows high of the contact angle.18,25,26 Our results demonstrate this,
chemical stability and resistance to acid corrosion.9 The as there was a significant decrease in the contact angle
search for a safe and efficient surface treatment for following nonthermal argon plasma application, thus
zirconia was the aim of this study. A surface treatment confirming Lopes et al,18 who reported the same findings
protocol for zirconia might eliminate the use of airborne- for zirconia.
particle abrasion, a procedure that damages the surface Commercially available primers can improve bond
of zirconia, leading to microcracks that might limit strength and change the contact angle to 30 or 40
restoration lifetime.7 Nonthermal argon plasma was degrees. by changing the inertia of the zirconia surface.
found to increase the bond strength to a similar extent to The decreased contact angle indicates that the surface
that produced by the standard treatment with airborne- became hydrophilic, thus increasing its potential of
particle abrasion, but without significantly altering sur- binding to adhesives, primers, and resin cements.18,25
face roughness, thus reducing the risk of fissures and Among the groups in which argon plasma was used
cracks. for bond strength testing, specimens were only ob-
An explanation for these results is that reactive atoms tained for those groups treated with 10% hydrofluoric
generated by the interaction of argon plasma ions and acid (HFNPP). As zirconia is a highly crystallized

THE JOURNAL OF PROSTHETIC DENTISTRY Vilas Boas Fernandes Júnior et al

- 2018
substrate (approximately 98% of its composition) and
consequently resistant to acid treatment,6 the applica-
tion of hydrofluoric acid before the plasma treatment
acted mainly to remove inorganic residue from the
cutting process and particles deposited from the at-
mosphere.8 Therefore plasma application was more
effective on the cleaned zirconia surface, resulting in bond
strength similar to the standard treatment with airborne-
particle abrasion. This finding could also be seen in the
spectral curves recorded with FTIR, which showed a sim-
ilarity in the curve patterns of both groups.
Treating zirconia with argon plasma is a cold process
in which no heat emission occurs, therefore there is little
risk of transformation of the tetragonal to the monoclinic
zirconia phase. However, phase transformation was not
evaluated, a limitation of this study. It should be a matter
for a future investigation. Further research is also needed
on longevity and also the efficacy of the treatment on
other ceramic systems. Improving the plasma devices for
clinical is also important.
CONCLUSIONS
Within the limitations of this in vitro study, the following
conclusions were drawn:
1. Nonthermal plasma application for surface treat-
ment of Y-TZP showed no significant difference in
bond strength when compared with airborne-
particle abrasion with Al2O3.
2. Nonthermal plasma application did not significantly
change the surface roughness pattern.
3. The contact angle of nonthermal plasma-treated
specimens was reduced compared with other sur-
face treatments.
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Corresponding author:
Dr Maria Filomena Rocha Lima Huhtala
Department of Restorative Dentistry
Institute of Science and Technology
São Paulo State University (UNESP)
Av, Engenheiro Francisco José Longo, 777
12245-000 São José dos Campos, São Paulo
BRAZIL
Email: huhtala@ict.unesp.br
Copyright © 2018 by the Editorial Council for The Journal of Prosthetic Dentistry.
THE JOURNAL OF PROSTHETIC DENTISTRY