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Keywords Abstract
Adhesives; PEEK; resin cement; shear bond
strength; surface roughness.
Purpose: To investigate the effect of various surface pretreatments and adhesive
systems on bond strength of resin cement to polyetheretherketone (PEEK).
Correspondence
Materials and Methods: 360 PEEK specimens were divided into 4 groups to receive
Ipek Caglar, Department of Prosthodontics, the following pretreatments (n = 90): no pretreatment, sandblasting, silica coating
Faculty of Dentistry, Recep Tayyip Erdogan and Er:YAG laser. Surface roughness (SR) and scanning electron microscopy (SEM)
University, Menderes St, No: 64, 53100, Rize, evaluations were conducted after mechanical pretreatments for topographical surface
Turkey. E-mail: ipeksatiroglu@hotmail.com evaluations. After the pretreatments, each group was divided into 3 subgroups (n = 30)
according to the adhesive system used: no adhesive system, Visio.link, and Signum
The authors deny any conflicts of interest. PEEK Bond. Resin cement was applied, and specimens underwent 5000 thermocycles
(5-55°C) before shear bond strength (SBS) test. One-way ANOVA and Tukey test
This study was orally presented at BASS
were used to analyze the SR data; 2-way ANOVA and Fisher’s LSD test were used to
Congress in Greece on 5–7 May 2017.
analyze the SBS data at the confidence interval of 95% (α = 0.05).
This study was supported by the Research Results: The sandblasting group demonstrated the highest SR values (p < 0.05).
Projects Fund of Recep Tayyip Erdogan No significant differences in SR values were identified among silica coating, laser,
University (Grant No: 2015.53001.111.08.04). and control groups (p ˃ 0.05). Conditioning with Visio.link after sandblasting group
exhibited the highest SBS values (p < 0.05). No significant differences in SBS values
Accepted February 4, 2018
were found between laser and control group (p ˃ 0.05). Conditioned groups presented
higher SBS values than unconditioned groups (p < 0.05). Between the two adhe-
doi: 10.1111/jopr.12791
sive systems, Visio.link demonstrated statistically significant higher SBS values than
Signum PEEK Bond (p < 0.05).
Conclusion: Silica coating and sandblasting were shown to provide superior pretreat-
ment of PEEK surface. Laser pretreatments showed no effectiveness on bond strength
of resin cement to PEEK. Adhesive systems improved the resin bonding to PEEK.
Polyetheretherketone (PEEK) is a high-performance thermo- was suggested for patients who exhibited nocturnal bruxism
plastic polymer that has superior chemical, thermal, and me- and clenching but refused to use an occlusal appliance.5
chanical properties and excellent biocompatibility.1 A modified Additional advantages of this polymer are elimination of
PEEK with 20% inorganic fillers has been used in dentistry for allergic reactions and metallic taste, high polishing qualities,
implants, temporary abutments for implant-supported prosthe- low plaque affinity, and good wear resistance.3-6 An in vivo
ses, healing abutments, implant-supported bars, clamp material, study reported that PEEK should probably be considered as an
or frameworks for removable and fixed partial prostheses.1-5 alternative removable partial denture framework material for
Among other thermoplastic polymers, PEEK absorbs less wa- patients with taste sensitivity or allergies to conventional Cr-Co
ter than polymethyl methacrylate (PMMA) and does not shrink frameworks.7 Although PEEK has significant advantages for
during the polymerization process like composite resin and dental applications, difficulties in establishing a strong and
PMMA. This material has low elastic modulus, which makes durable adhesion to dental material are the major clinical
it as elastic as bone and allows it to act as a stress breaker and disadvantage.1,2,9 Current studies focus on enhancing PEEK
reduce forces transferred to the restorations.2,3 surface for reacting with resins to allow bonding, because the
Zoidis4 evaluated these properties in vivo and recommended clinical performance of fixed dental prostheses mainly relies
PEEK implant frameworks in combination with prefabricated on the luting procedure.2,3,8,9 Generally, two methods to obtain
high-impact PMMA veneers for an alternative treatment a strong bonding performance between the resin cement and
for All-on-4 implant restorations. PEEK crown framework PEEK have been the focus of recent studies: the alteration of
PEEK breCAM.BioHPP Bredent GmbH & Co KG PEEK, 20% weight titanium oxide 420212
Aluminum oxide Cobra Renfert GmbH Aluminum oxide sand (50 μm mean 15941205
particle size)
Tribochemical The CoJet system 3M ESPE Silicatized sand (30 μm mean particle 625642
silica coating size)
Adhesive Visio.link Bredent GmbH & Co KG MMA, pentaerythritol triacrylate, photo 142655
system initiators
Adhesive Signum PEEK Bond Heraeus Kulzer GmbH Bond I: Bifunctional molecules based Bond
system on phosphoric acid esters and thiol I: 10133
compounds; Bond
Bond II: MMA, PMMA, photoinitators II:
010500
Resin cement Panavia SA Cement Plus Kuraray Noritake Paste A: MDP, Bis-GMA, TEGDMA, B40206
Dental Inc. hydrophobic aromatic dimethacrylate,
HEMA;
Paste B: Hydrophobic aromatic
dimethacrylate, hydrophobic aliphatic
dimethacrylate
PEEK: Polyetheretherketone, MMA: Methylmethacrylate, PMMA: Polymethylmethacrylate, Bis-GMA: Bisphenol A diglycidylmethacrylate, MDP: Methacryloy-
loxydecyl dihydrogen phosphate, TEGDMA: Triethyleneglycol dimethacrylate, HEMA: Hydroxymethacrylate.
the PEEK surface and conditioning with an adhesive system to treatments provide more functional groups to which the com-
enable the chemical interactions.9,10 ponents of adhesive systems can bond.16,22
Several studies have examined the bond strength between All PEEK studies have reported that bonding to PEEK must
resin and PEEK material by various pretreatments such as sand- be improved to achieve adequate, long-term adhesion clini-
blasting, silica coating,11,12 treating the surface with piranha cally; however, information concerning the potential and lim-
etching,2,13 sulfuric acid,14,15 or different types of plasma.16 itations of PEEK in bonding to dental material is still insuffi-
Studies have found that sandblasting improves the bond cient. Therefore, the aim of this study was to evaluate the effect
strength between resin and PEEK material and propose this of mechanical pretreatments and adhesive systems on the bond
as one of the best initial pretreatment alternatives for PEEK strength of resin cement to PEEK. The null hypotheses were
surfaces.11,14,17 Rosentritt et al18 reported that tribochemical that PEEK surface pretreatments or conditioning with adhe-
treatment might be an alternative pretreatment on PEEK sur- sives would have no effect on the bond strength values between
faces to achieve successful bonding; however, to our knowl- PEEK and resin cement.
edge, there are relatively few reports on material processing
and no reports on PEEK surface treatment with lasers. Er:YAG
laser is a commonly used laser system for surface treatment Materials and methods
of dental materials.19-21 However, there is no consensus in the Specimen preparation
literature about the laser parameters for optimal bond strength
of resin-based materials. The compositions and details of the materials used in this study
Surface pretreatments arrange the PEEK surface for mi- are shown in Table 1. Three hundred and sixty disk-shaped
cromechanical bonding to resin; however, additional adhesives PEEK specimens were milled from a prefabricated blank
are essential in establishing a strong bond between PEEK and (breCAM.BioHPP; Bredent GmbH, Senden, Germany). These
resin. Most studies reported that adhesive systems that contain specimens were embedded in an autopolymerizing acrylic resin
methylmethacrylate (MMA) were able to constitute a sufficient (Meliodent; Heraeus Kulzer GmbH, Hanau, Germany), and the
bond to PEEK.8-10,12 Studies showed that the combination with bonding surfaces of each specimen were polished with 600-
pretreatments enhances the bond strength because mechanical and 800-grit silicon carbide paper under running water. Then,
the specimens were cleaned in an ultrasonic cleaner (Eurosonic
E4D; Euronda, Vicenza, Italy) for 10 minutes with distilled Table 2 Classification of specimens in test groups with respect to pre-
water and air dried before surface treatment. treatments and adhesive systems used
Figure 2 Surface topography of untreated PEEK surface (2000×). Figure 5 Surface topography of sandblasted PEEK surface (2000×).
Group Mean ± SD
C 1.11 ± 0.09a
B 2.64 ± 0.28b
S 1.20 ± 0.17a
L 1.19 ± 0.20a
Table 4 Mean and standard deviation for shear bond strength values of test groups (MPa)
Failure mode
C No adhesive 30 0 0 30
Visio.link 18 0 12 30
Signum PEEK Bond 19 0 11 30
B No adhesive 22 0 8 30
Visio.link 11 0 19 30
Signum PEEK Bond 21 0 9 30
S No adhesive 27 0 3 30
Visio.link 14 0 16 30
Signum PEEK Bond 23 0 7 30
L No adhesive 30 0 0 30
Visio.link 30 0 0 30
Signum PEEK Bond 30 0 0 30
active surface layer by removing organic contaminant from bond strength values than Signum PEEK Bond (p < 0.05).
the material surface, and advances micromechanical interlock- The differences between the two systems may be related to the
ing of polymer-based dental materials.9,11,24 Previous stud- chemical composition of adhesives or pretreatments applied be-
ies reported a significant increase in SBS values after sand- fore conditioning. Signum PEEK Bond comprises MMA and
blasting compared to nonpretreated PEEK due to variation of bifunctional monomers based on phosphoric acid esters; how-
surface morphology.9,14,15,17,18 In agreement with previous ever, the main constituents of Visio.link are MMA and PETIA
studies, in this study, the specimens sandblasted with 50 μm (pentaerythritol triacrylate). Because of PETIA’s high capacity
Al2 O3 showed significantly higher SR (2.64 ± 0.28 μm) and to modify the PEEK surface, Visio.link provided higher bond
SBS (11.65 ± 2.09 MPa) values than the control group. High strength values to PEEK restorations. Despite this study, previ-
SBS values of the sandblasting group are related to the topog- ous studies stated that both Visio.link and Signum PEEK Bond
raphy of treated surfaces by sandblasting, because irregularities increased the bond strength values significantly, and there were
in the bonding area increase the contact area for the material no differences between them.2,9 The differences of these stud-
to bond with. SEM images verified this view that an irregu- ies may contribute to the pretreatments used before condition-
lar fissure pattern with larger grooves is more suitable for the ing. These studies used strong acids for modifying the PEEK
flow of both adhesive and resin cement, as observed with sand- surface; however, only mechanical pretreatments were used in
blasted PEEK specimens (Fig 5). Additionally, alumina powder this study. Also, Uhrenbacher et al9 evaluated the veneering
inserted in the PEEK surface may interfere with the application composite resin bonding to PEEK, whereas we evaluated self-
of bonding. adhesive resin cement.
Silica coating is another surface pretreatment option for dif- In the current study, the highest SBS values were shown
ferent dental material surfaces such as composite or ceramic. in specimens conditioned with Visio.link in the sandblasting
The CoJet system consists of 30 μm Al2 O3 particles sand coated group (19.86 ± 2.52 MPa). Kern and Lehmann26 also reported
with SiO2 incorporated into the PEEK surface to improve the only multifunctional methacrylate containing adhesive systems
bonding of resin during this process. Schmidlin et al11 evalu- on sandblasted PEEK surfaces promising durable bonding to
ated the bonding potential of pretreated PEEK surfaces to resin PEEK. Another study also corroborated these finding and noted
and reported that silica coating (11.5 ± 3.2 MPa) significantly that conditioning the PEEK surface with MMA-containing
increased the SBS values. Although there were no significant adhesive systems after silica coating or sandblasting increased
differences in SR values between silica coating and the con- the SBS values.15 Stawarczyk et al12 noted that Visio.link
trol group, silica-coated (9.59 ± 1.58 MPa) PEEK specimens acted as the positive control group, because all previous
exhibited higher SBS values than the control group (5.58 ± studies showed very high bonding properties after the use
0.38 MPa) in the current study. Rosentritt et al18 reported that of Visio.link as conditioner on different pretreated PEEK
roughening of the surface alone with pretreatments was not suf- surfaces, and recommended sandblasting as one of the best
ficient to guarantee a stable bonding between resin cement and initial pretreatment options for PEEK surfaces.12,16,18,21 Thus,
PEEK surface. In addition, they posited that surface topography the current findings are not surprising.
and conditioning of the surface were more crucial for bonding The conditioned laser group exhibited higher SBS values
procedure than SR. In this study, SEM evaluation clearly dis- than the unconditioned laser group in this study. Although a
played irregularities and silica particles on the PEEK surface. statistically significant increase was found in conditioning with
Most probably the silica particles and modified surface mor- Visio.link, Signum PEEK Bond had no statistically significant
phology enhance the initial bonding with self-adhesive resin effect on SBS for laser (p > 0.05). The results showed that
cement. adhesive effectiveness on laser was lower than other pretreat-
To the knowledge of the authors, this is the first evaluation ments. The surface morphology after laser treatments may be
of the effect of laser application on bonding performance of the reason for low SBS values. Laser-treated PEEK surfaces
resin cement to PEEK. For this reason, the results of this study represent a complicated structure, and resin cement may not
cannot be compared to other available studies. There were no flow onto the material (Fig 3). Furthermore, the physical prop-
significant differences found in SR and SBS values between erties of the bonding area are important for the bonding process.
the laser and control groups. In addition, the SEM image of If the laser creates a moisture surface after application, adhesive
laser-treated PEEK surfaces displayed a complicated structure penetration would be troubled because methacrylate in the ad-
with deeper and narrow pits, which make the flow of resin hesive system is hydrophobic, and sufficient bonding would not
materials difficult (Fig 3). be achieved on the moisture surface. Hence, additional studies
Generally, dental adhesives are used to improve bonding are required to investigate the physical properties after laser
of inert PEEK surface to resin. The bonding success between pretreatment and should focus on laser parameters.
PEEK and resin is related to the content and solvents of the ad- The acceptable SBS value at the interface of resin-based ma-
hesive system. Previous studies found that adhesive systems terial and framework is 5 MPa according to the requirements
that contain MMA monomers caused higher bond strength of ISO 10477.23 However, the minimum clinical SBS value of
values between PEEK and resin.15,16,18,25 For this reason, Vi- resin-based material under oral conditions has been reported to
sio.link and Signum PEEK bond were chosen for adhesive be 10 to 12 MPa.27,28 In this study all tested specimens were
systems in this study. With regard to the adhesive systems, found to be within the range of ISO 10477,23 but clinical re-
Visio.link and Signum PEEK Bond led to an increase in SBS quirements for SBS values cannot be reached in the control and
values for all pretreatment groups; however, the Visio.link adhe- laser treatment group. Thus, the results of this study demon-
sive system demonstrated statistically significant higher shear strated that PEEK crown should be sandblasted with 50 μm
Al2 O3 particle or silica coated before cementation for improved 5. Zoidis P, Bakiri E, Papathanasiou I, et al: Modified PEEK as an
bonding. Nontreated PEEK surface should be conditioned by alternative crown framework material for weak abutment teeth: a
MMA containing adhesives before cementation. case report. Gen Dent 2017;65:37-40
SBS tests are more suitable for evaluating the adhesive ca- 6. Siewert B, Parra M: A new group of material in dentistry. Peek as
pabilities of resin-based materials. Any changes in the surface a framework material used in 12-piece implant-supported
bridges. Z Zahnarzt Implantol 2013;29:148-159
features of the tested material may affect the SBS values, which
7. Zoidis P, Papathanasiou I, Polyzois G: The use of a modified
are related to chemical and mechanical adhesion.24,29 However, poly-ether-ether-ketone (PEEK) as an alternative framework
a high amount of adhesive failures occurred in this study be- material for removable dental prostheses. A clinical report. J
cause the bond strength of resin cement to PEEK was not suffi- Prosthodont 2016;25:580-584
ciently high.24 The mixed failure is mainly due to the irregular 8. Bauer J, Costa JF, Carvalho CN, et al: Influence of alloy
distribution of the shear forces at the resin/PEEK interface. microstructure on the microshear bond strength of basic alloys to
The aging consisted of thermocycling for 5000 thermal cy- a resin luting cement. Braz Dent J 2012;23:490-495
cles (5°C/55°C; dwell time, 20 seconds), which corresponds 9. Uhrenbacher J, Schmidlin PR, Keul C, et al: The effect of surface
to approximately 4 to 5 years clinical service.16 The effect of modification on the retention strength of polyetheretherketone
thermocycling on the SBS of resin cement to pretreated PEEK crowns adhesively bonded to dentin abutments. J Prosthet Dent
2014;112:1489-1497
specimens plays an important role in long-term predictability,
10. Marshall SJ, Bayne SC, Baier R, et al: A review of adhesion
because studies have shown that intraoral thermal changes are science. Dent Mater 2010;26:11-16
easily simulated by using the thermoycling method.9,16,30 In 11. Schmidlin PR, Stawarczyk B, Wieland M, et al: Effect of
this way, all tested specimens received a standardized and re- different surface pre-treatments and luting materials on shear
producible thermal stress, but there is no systematic standard bond strength to PEEK. Dent Mater 2010;26:553-559
procedure for subjecting materials to thermocycling regimens 12. Stawarczyk B, Taufall S, Roos M, et al: Bonding of composite
at present. resins to PEEK: the influence of adhesive systems and
This study has some limitations. Only one type of laser pa- air-abrasion parameters. Clin Oral Investig 2018;22:763-771
rameter was used. Different lasers and laser parameters for 13. Hallmann L, Mehl A, Senero N, et al: The improvement of
resin bonding to PEEK must be further investigated. Although adhesive properties of PEEK through pretreatments. Appl
Surface Sci 2012;258:7213-7218
conventional and resin cements are used for the cementation of
14. Stawarczyk B, Beuer F, Wimmer T, et al:
PEEK based restorations, in this study only resin cement was Polyetheretherketone—a suitable material for fixed dental
evaluated. Additional comparative studies with different lut- prostheses? J Biomed Mater Res B Appl Biomater
ing cements are recommended. All specimens were produced 2013;101:1209-1216
and evaluated under in vitro conditions, so this study cannot 15. Stawarczyk B, Keul C, Beuer F, et al: Tensile bond strength of
reflect the conditions of clinical applications exactly. Further veneering resins to PEEK: impact of different adhesives. Dent
structured in vivo studies are necessary for clinical assessment. Mater J 2013;32:441-448
16. Stawarczyk B, Bahr N, Beuer F, et al: Influence of plasma
pretreatment on shear bond strength of self-adhesive resin
Conclusions cements to polyetheretherketone. Clin Oral Investig
2014;18:163-170
Within the limitations of this in vitro study: 17. Sproesser O, Schmidlin PR, Uhrenbacher J, et al: Effect of
sulfuric acid etching of polyetheretherketone on the shear bond
1. Silica coating and sandblasting demonstrated the highest
strength to resin cements. J Adhes Dent 2014;16:465-472
SBS values among the pretreatments applied to PEEK. 18. Rosentritt M, Preis V, Behr M, et al: Shear bond strength
2. 1.5 W (150 mJ) Er:YAG laser pretreatment of PEEK between veneering composite and PEEK after different surface
surface did not influence the bonding effectiveness of modifications. Clin Oral Investig 2015;19:739-744
resin cement. 19. Akın H, Ozkurt Z, Kırmalı O, et al: Shear bond strength of resin
3. Adhesives improved the bond strength of PEEK restora- cement to zirconia ceramic after aluminum oxide sandblasting
tions with or without surface pretreatments. and various laser treatments. Photomed Laser Surg
4. The SEM evaluations showed that surface topography 2011;29:797-802
affects the adhesion more than surface roughness. 20. Akin H, Tugut F, Akin GE, et al: Effect of Er:YAG laser
application on the shear bond strength and microleakage between
resin cements and Y-TZP ceramics. Lasers Med Sci
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