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Table of Contents   
Year : 2023  |  Volume : 26  |  Issue : 3  |  Page : 281-287
Influence of nonthermal argon plasma on the micro-shear bond strength between resin cement and translucent zirconia

1 Department of Prosthodontics, School of Dentistry, Tehran University of Medical Sciences, Tehran, Iran
2 Dental Research Center, Dentistry Research Institute, Department of Prosthodontics, School of Dentistry, Tehran University of Medical Sciences, Tehran, Iran
3 Department of Oral Biological and Medical Sciences, University of British Columbia, Faculty of Dentistry, Vancouver, BC, Canada
4 Department of Periodontics and Oral Medicine, School of Dentistry, University of Michigan, Ann Arbor, MI, USA

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Date of Submission14-Jan-2023
Date of Decision31-Jan-2023
Date of Acceptance02-Mar-2023
Date of Web Publication16-May-2023


Background: Considering the potential of translucent zirconia for application in esthetic restorations, it is necessary to find effective methods with the least adverse effects to increase its bond strength to resin cement.
Aims: This study aimed to test if different conservative surface treatments and cement types could affect the micro-shear bond strength (μSBS), failure mode, and bonding interface between resin cement and translucent zirconia.
Materials and Methods: In this in vitro experimental study, translucent zirconia blocks were divided into four groups based on the surface treatment they received: no treatment, argon plasma, primer (Pr), and Pr + plasma. Each group was further divided into two subgroups based on the applied cement: PANAVIA F2 and Duo-Link cement. Fourteen cement columns with a diameter of 1 mm were placed on each block (n = 14); all the specimens were immersed in 37°C water for 24 h. Afterward, μSBS was evaluated (P < 0.05), and the mode of failure was determined by a stereomicroscope (×10). The cement–zirconia interface and the surface hydrophilicity (contact angle) were also evaluated.
Statistical Analysis: Two-way analysis of variance (ANOVA) was used to evaluate the effect of surface preparation, cement types, and incubator, simultaneously (P < 0.05). The bond strengths after incubation were analyzed by one-way ANOVA (P < 0.05). Failure mode, contact angle, and cement–zirconia interface were analyzed descriptively.
Results: The highest bond strength was seen in Pr surface treatment for Duo-Link cement; however, this group was not significantly different from Pr and PANAVIA F2 cement and Pr + plasma and Duo-Link cement (P = 0.075) groups. All plasma specimens in the incubator failed prematurely. The mode of failure in all specimens was adhesive. The lowest and highest contact angles were seen in Pr + plasma and the control groups, respectively.
Conclusion: The use of Pr could successfully improve the bond strength of resin cement to translucent zirconia while plasma was not an acceptable and durable substitute.

Keywords: Adhesive; esthetic; plasma; resin cement; zirconium oxide

How to cite this article:
Salimi K, Atri F, Valizadeh S, Sahebi M, Ghodsi S, Manouchehri N. Influence of nonthermal argon plasma on the micro-shear bond strength between resin cement and translucent zirconia. J Conserv Dent 2023;26:281-7

How to cite this URL:
Salimi K, Atri F, Valizadeh S, Sahebi M, Ghodsi S, Manouchehri N. Influence of nonthermal argon plasma on the micro-shear bond strength between resin cement and translucent zirconia. J Conserv Dent [serial online] 2023 [cited 2023 Dec 8];26:281-7. Available from:

   Introduction Top

Zirconia ceramic has high mechanical properties and considering its chemical stability, acceptable esthetic, high fracture resistance, and biocompatibility, tetragonal zirconia has become a fascinating substitute for alloys as restorative core material. However, the opaque appearance encouraged the companies to find more esthetically appealing types. Translucent zirconia was introduced in 2011[1] and expanded the scope of zirconia applications to full contour esthetic restorations. However, the bond between zirconia and resin cement has physically challenged the application of this ceramic in partial coverage esthetic restorations.[2]

Various physical and chemical methods were introduced to overcome this problem. Surface preparation of zirconia was tried by air abrasion, silica coating,[3] application of phosphate monomers[4] chemical etching (by hydrofluoric acid),[5] laser application (by neodymium-doped: Yttrium Aluminum Garnet [Nd: YAG], CO2, and Erbium-doped: YAG lasers),[6],[7] and plasma.[8] Despite all the research, none of these methods could provide completely reliable results without adverse side effects. Sandblasting, as one of the most effective surface treatments, could change the surface chemical properties by alumina particle contamination, and increase the risk of zirconia cracking, margin deformation, and chipping.[9],[10] Moreover, the findings of some in vitro studies indicate the microcracks and gross surface defects after the sandblasting process in zirconia.[11],[12] Laser application could provoke cracking in the ceramic and pave the way for future failures.[13] However, according to Kermanshah[14] by increasing the surface irregularities, the use of Nd: YAG laser increases the bond strength between zirconia and dentin. Surface treatment by a combination of sandblasting and using 10-methacryloyloxydecyl dihydrogen (10-MDP)-based primers (Prs) have shown more acceptable results; however, the aging process might affect the bond durability between the sandblasted surface and MDP-based materials.[15] According to Tayal,[16] 10-MDP-based universal adhesives together with sandblasting can increase 24-h shear bond strength between zirconia and resin.

Nonthermal plasma (NTP) could be a viable alternative to previous surface treatment methods. NTP consists of a semi-ionized gas in an unbalanced environment that produces a considerable amount of chemically active groups such as H2O2, OH, O3, NO, and OH radicals at low temperatures[17] and convert an inert surface into a reactive one with increased energy without changing the substance properties.[18]

Given the potential of translucent zirconia for application as partial coverage esthetic restoration, it would be necessary to find an acceptable surface treatment that provides a reasonable bond without putting the polycrystalline ceramic at an increased risk of fracture.

This study aimed to test if different conservative surface treatments (using active monomer, argon plasma, or combination) and cement types (with or without 10-MDP) could affect the micro-shear bond strength (μSBS), failure mode, and bonding interface between resin cement and translucent zirconia. The argon gas was chosen for plasma treatment since it is the most common inert gas used to increase bond strength, and its ionization energy and cost are low.[19],[20] The null hypotheses were that there will be no significant differences in the bond strength and failure mode between evaluated groups; the failure would be mainly adhesive, and the surface hydrophilicity and interface are almost the same in all the surface treatments.

   Materials and Methods Top

Sample size determination

According to the results of Ito study[19] and considering α =0.05, β =0.2, the effect size of 0.15, and a standard deviation of 3.5 MPa, the minimum sample size required was 14.

Specimen preparation

This in vitro study was performed on monolithic high translucent zirconia (Incoris TZI mono L F0, Dentsply Sirona, New York, United States). The initial blocks were cut into 20 mm × 19 mm × 2 mm blocks (Mecatome T201, Presi, Grenoble, France) and sintered (inFire HTC speed, Dentsply Sirona, New York, United States) according to the manufacturer's instructions. The surface of the specimens was polished with abrasive papers (Matador 991A softflex, Germany) for 1 min. The blocks were put in ultrasonic (Eurosonic 4D, Euronda, Italy) for 6 min, cleaned with 96% ethanol, and divided into four groups (n = 28) based on the surface treatment they received [Figure 1].
Figure 1: Interface between cement and zirconia by SEM at 1000 (left images: 1) and 3000 (right images: 2) magnifications. (a) Panavia and untreated zirconia, (b) Duo-Link and untreated zirconia, (c) Panavia and plasma-treated zirconia, (d) Duo-Link and plasma-treated zirconia, (e) Panavia and primer-treated zirconia, (f) Duo-Link and primer-treated zirconia, (g) Panavia and primer + plasma-treated zirconia, (h) Duo-Link and primer + plasma-treated zirconia

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  • Group 1: Without any surface treatment, played the role of the control group (C)
  • Group 2: Z-Prime Plus Pr (Bisco, Atlanta, United States) was evenly applied on the surface and gently dried for 3–5 s (Pr)
  • Group 3: The blocks were irradiated by NTP (Nik Technavran Plasma, Medaion Plasma Therapy Device Model S, Tehran, Iran) from a distance of 10 mm for 45 s using argon gas in a voltage of 5 kV and a flow rate of 3000 sccm (NTP)
  • Group 4: Z-Prime plus Pr was applied to the blocks and after drying, they were irradiated with NTP using argon gas (Pr + NTP).

Micro-shear bond strength test

Each group was divided into two subgroups based on the selected cement for the μSBS test (n = 14 for each subgroup). In the first subgroup, a self-etching cement (PANAVIA F2, Kuraray, Tokyo, Japan) containing (10-MDP) and in the second subgroup, a total-etch cement (Duo-Link, Bisco, United States, Chicago) without MDP content was used. Fourteen Tygon tubes with an inner diameter of 1 mm and a height of 2 mm were used to place the cement specimens on each zirconia block. After mixing, the cement was placed and irradiated for 5 s (LED. D, Woodpecker, China), the excess cement was removed, and irradiation was completed for 20 s from the opposite side of each zirconia block. The light intensity was 1000 mW/cm2, and the intensity of radiation was checked every 5 s using a radiometer.

The first set of μSBS tests was performed on all the groups (except Pr + NTP) without placing them in the incubator. Afterward, all the samples were immersed in 37° distilled water for 24 h (wet incubator, Kavosh Mega, Tehran, Iran). Each block was connected to a universal testing machine (Zwick Roell, Ulm, Germany) by 0.3-mm stainless steel wire to measure the μSBS by loop methods. The shear force of 0.5 mm/min was applied until failure occurred which was recorded in newtons. The μSBS in MPa was calculated by dividing the force in newtons by the contact surface of the cylinder.

Failure mode

Direct view by stereomicroscope (Olympus, SZX9, Japan) at × 10 magnification was used to determine the mode of failure that was expected to be in three different types: Cohesive failure that occurs within resin cement (or zirconia), adhesive failure that occurs between cement and zirconia, and mixed failure or a combination of both failure modes.[21]

Contact angle

The hydrophilicity was measured by a contact angle meter after dropping three drops of distilled water (approximately 10 μl) on each experimental block at room temperature.

Interface between cement and zirconia (scanning electron microscope analysis)

Two samples of each resin cement were placed on each experimental block using a plastic tube with a 4-mm diameter. After curing and mounting the samples in acrylic, the blocks were cut using mecatome and evaluated by scanning electron microscope (SEM) (FEI Nova NanoSEM450, FEI, Oregon, United States) in magnification of 1000 and 3000.

Statistical analysis

Two-way analysis of variance (ANOVA) was used to evaluate the effect of surface preparation, cement types, and incubator, simultaneously (P < 0.05). The bond strengths after incubation were analyzed by one-way ANOVA (P < 0.05). Failure mode, contact angle, and cement–zirconia interface were analyzed descriptively.

   Results Top

Micro-shear bond strength

[Table 1] describes the μSBS of cement in various zirconia surface treatments with and without incubation. Two-way ANOVA was performed between the groups for which, data were available before and after incubation to evaluate the effect of surface treatments, different cement, and incubation, simultaneously, with a significance limit of P < 0.05.
Table 1: Micro-shear bond strength of Duo-Link and PANAVIA F2 cement in different surface treatments with and without incubation

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The interaction between groups and the incubator was not significant (P = 0.073). The results were different between the groups with or without incubation and the incubation affected the results significantly in all the groups. Therefore, the pilot study results (without incubation) were merged with the results obtained after incubation to increase the study power. [Table 2] summarizes the P value comparisons between different surface treatments in two cement groups. After incubation, there was no significant difference between PANAVIA F2 and Duo-Link cement in each of the study groups including control (P > 0.099), plasma (P > 0.099), Pr (P = 0.162), and Pr + plasma (P = 0.497). The highest μSBS after incubation for Duo-Link cement was seen in Pr surface treatment (11.13 Mpa) that was followed by Pr + plasma (6.25 Mpa), control (1.05 Mpa), and plasma (0 Mpa) groups. In PANAVIA cement, the reducing sequence were Pr (6.81 Mpa), Pr + plasma (2.98 Mpa), control (0.45 Mpa), and plasma (0 Mpa) groups, respectively.
Table 2: P value comparison of different surface treatments for PANAVIA F2 and Duo-Link cement

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Failure mode

The failure modes were adhesive in all the specimens. [Figure 1] shows the interface between cement and zirconia surfaces in different study groups.

Interface between cement and zirconia (scanning electron microscope analysis)

According to interface analysis, Duo-Link cement, generally, showed more entanglement (less gap) in cement–zirconia interface compared to Panavia groups. In Duo-Link groups, in groups D (plasma-treated zirconia) and H (Pr + plasma-treated zirconia), more entanglement could be seen in the interface.

Contact angle

In the contact angle evaluation, the highest contact angle was seen in the control group (64.9°) while the lowest was related to the Pr + plasma group (28.4°); on the other hand, Pr + plasma surface treatment caused more hydrophilicity and wettability of zirconia surface. [Figure 2] shows the contact angle measurements in study groups.
Figure 2: Contact angle measurements in study groups.(a) zirconia without treatment (64.9°(, (b) zirconia treated by plasma (31.7°), (c) zirconia treated by primer (36.7°), (d) zirconia treated by primer + plasma (28.4°)

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   Discussion Top

The introduction of translucent zirconia has extended the range of zirconia applications; however, the adhesive bond between zirconia and resin cement is still one of the challenges of using this glass-free ceramic. A proven method of bond improvement, the use of the sandblast-Pr combination,[22],[23] has a high probability of phase change and crack formation[9],[10] that has prompted researchers to look for alternative methods. On the other hand, the effect of alternative methods has been, mainly, evaluated on tetragonal zirconia, while the translucent types have the potential to be used in esthetic partial coverage restorations that depend on adhesive bonding for retention. This study compared the effect of Pr, plasma, and combination treatments on surface hydrophilicity, bond strength, and interface of two different types of resin cement.

The null hypotheses were partially rejected since there were significant differences between the bond strength of evaluated groups, and also different surface treatments affected the contact angles and interfaces. However, the failure modes were all adhesive. The highest μSBS after 24 h of incubation was seen in the Pr group, followed by the Pr + plasma group. The same results were reported by Vechiato-Filho et al.[24] and Kaimal et al.[25] while Valverde et al. reported higher bond strength by Pr + plasma treatment.[26]

Plasma application reduced the contact angle in plasma and Pr + plasma groups. The surface of zirconia is highly hydrophobic with a low concentration of OH groups.[27],[28] NTP could increase surface energy.[26] During plasma application, the moisture in the gas and atmosphere combines with the high-energy electrons of the surface to produce OH radicals. Plasma also breaks the bonds between C-C and C-H in organic impurities attached to the zirconia[19],[20] resulting in the formation of activated peroxide radicals and increasing the composition of functional groups (e.g., C-O and C-OH) on the surface.[29] Increasing the polar composition of oxygen increases the hydrophilicity of the surface[24],[30] as seen in the present study by contact angle reduction. NTP has been reported to promote the formation of secondary intermolecular forces such as Van der Waals bonds between hydroxyl groups on the surface and resin cement.[26],[29] The present study results before incubation confirms the effect of plasma in increasing the bond strength and are in line with the results of other studies.[20],[22],[25],[31] However, after incubation, premature failure occurred in all the specimens treated by plasma inside the incubator. This result shows the low resistance of Van der Waals bonds to hydrolysis and thermal stresses.[32],[33]

The highest bond strength was seen in Pr-treated zirconia. Z-Prime contains 10-MDP. The main chemical bonds established between 10-MDP and zirconia include ionic, metallic, covalent, and chelation bonds.[34] Z-Prime also contains organophosphate and carboxylate monomers. Organophosphate consists of a functional part (usually a methacrylate group) that can be copolymerized with the monomers of resin cement.[35],[36] This Pr also contains functional phosphate and carboxylate monomers that can bond with metal oxides in the substrate to improve bonding.[37] The same results have been reported by Filho et al.[24], Valvarde et al.[26], Ahn et al.[22] and Negreiros et al.[38] In the other group of the present experiment, after applying the Pr, the surface of zirconia was treated with plasma. The results of μSBS in this group were higher than the control and plasma groups and lower than the Pr group. This weakening effect returns to the formation of active peroxides (R-O-O) and increases in functional compounds (C-O and C-OH) on the surface.[20],[39] These changes after plasma application can affect the interaction between hydroxyl groups in the Pr and zirconia and reduce the effect of the Pr on improving bond strength. The controversies in literature[19],[22],[25],[26],[31] confirm the technique sensitivity of plasma application, and the effect of gas type and purity, and plasma system on the obtained results.

In the present study, two types of resin cement were used; Duo-Link cement, produced by Bisco, is a Bis-GMA-based cement, and PANAVIA F2 cement, produced by Kuraray, contains MDP monomer. Previous studies introduced resin cement containing MDP as the most suitable cement for bonding with zirconia. This effect relates to the chemical interaction between the hydroxyl groups of the passive zirconia surface and the MDP phosphate ester group.[40] In this study, MDP containing Pr increased the bond strength with both types of cement, but contrary to the expectations, there was no significant difference between the two types of resin cement. The reason could be related to the methacrylate-based monomers in Duo-Link cement, which react directly with the organofunctional in the Pr to form a stable bond.[41] On the other hand, the higher filler content in PANAVIA F2 cement[42] could reduce the penetration depth in this cement. Furthermore, MDP-containing cement is highly dependent on the curing process for complete polymerization, since the functional acid monomer (MDP) reacts with the amine initiator and reduces the rate of chemical polymerization.[43] The opaque nature of zirconia might prevent complete penetration of light in the whole ceramic thickness. SEM images taken from the interface in the present study could also confirm the better performance of Duo-Link cement. However, Karimipour-Saryazdi et al.[44] reported higher bond strength for MDP-based cement (PANAVIA F2) compared to non-MDP type (Duo-Link). This controversy calls for further research.

According to stereomicroscopic images, all failure modes were adhesive that occurred in the interface between cement and zirconia. This result further emphasizes the low bond strength between resin cement and translucent zirconia in all the surface treatments made.

Considering the results of the present in vitro study, further research is encouraged with different plasma gas and varieties of times to find more acceptable methods that could provide a strong and durable bond between translucent zirconia and resin cement so that this ceramic option could be used with confidence in partial coverage esthetic restorations. Since in self-etch adhesive systems, contamination with saliva and blood can significantly reduce the bond strength,[45] it is necessary to conduct more studies by reconstructing the intraoral conditions.

   Conclusion Top

Considering the limitations of this experimental study, the following conclusions could be made:

  1. The surface treatment with NTP increased the bond strength compared to “no treatment,” but this bond was unstable and could not withstand moisture
  2. The use of nonthermal argon plasma did not provide stable and durable bond strength between translucent zirconia and resin cement
  3. MDP-contained Pr could increase the μSBS significantly in both cement
  4. The highest bond strength was seen in the group treated by the Pr in the application of two types of resin cement
  5. Pr + plasma treatment increased the surface hydrophilicity, followed by plasma treatment.


The authors would like to thank the vice chancellery of Tehran University of Medical Sciences and Health Services, Tehran, Iran, for supporting the research (Grant no: 99-2-133-48607). This study is pertinent to the DDS thesis of Dr. Kimia Salimi (#6613). The authors also thank Dr. Mohammadjavad Kharazifard for his assistance in statistical analysis, and Dr. Hamed Nikmaram for his scientific and technical support.

Financial support and sponsorship


Conflicts of interest

There are no conflicts of interest.

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Correspondence Address:
Dr. Safoura Ghodsi
Associate Professor, Dental Research Center, Dentistry Research Institute, Department of Prosthodontics, School of Dentistry, Tehran University of Medical Sciences, North Kargar St, Tehran
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Source of Support: None, Conflict of Interest: None

DOI: 10.4103/jcd.jcd_41_23

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