materials
Article
Comparative Evaluation of Tensile Bond Strength of Poly Ether
Ether Ketone (PEEK) and Zirconia Copings Using Resin Cement
with or without Adhesive: An In Vitro Study
Nimisha Kakkad 1, *, Naveen S. Yadav 1 , Puja Hazari 1 , Shweta Narwani 1 , Kirti Somkuwar 1 , Sakeenabi Basha 2 ,
Varsha Verma 1 , Suraj Arora 3 , Omir Aldowah 4, *, Artak Heboyan 5 and Mohmed Isaqali Karobari 6,7
Citation: Kakkad, N.; Yadav, N.S.;
Hazari, P.; Narwani, S.; Somkuwar,
K.; Basha, S.; Verma, V.; Arora, S.;
Aldowah, O.; Heboyan, A.; et al.
Comparative Evaluation of Tensile
Bond Strength of Poly Ether Ether
Ketone (PEEK) and Zirconia Copings
Using Resin Cement with or without
Adhesive: An In Vitro Study.
Materials 2022, 15, 4167. https://
doi.org/10.3390/ma15124167
Academic Editor: Bongju Kim
Received: 4 May 2022
Accepted: 10 June 2022
Published: 12 June 2022
Publisher’s Note: MDPI stays neutral
with regard to jurisdictional claims in
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iations.
Copyright: © 2022 by the authors.
Licensee MDPI, Basel, Switzerland.
This article is an open access article
distributed under the terms and
conditions of the Creative Commons
Attribution (CC BY) license (https://
creativecommons.org/licenses/by/
4.0/).
Materials 2022, 15, 4167. https://doi.org/10.3390/ma15124167
1 Department of Prosthodontics Crown & Bridge and Implantology, Peoples Dental Academy, Peoples
University, Bhopal 463027, India; naveensyadav@gmail.com (N.S.Y.); drhazaripooja@gmail.com (P.H.);
drshwetanarwani@gmail.com (S.N.); drkirtisomkuwar@gmail.com (K.S.); varshaverma1987@gmail.com (V.V.)
2 Department of Community Dentistry, Faculty of Dentistry, Taif University, P.O. Box 11099,
Taif 21944, Saudi Arabia; sakeena@tudent.edu.sa
3 Department of Restorative Dental Sciences, King Khalid University, P.O. Box 960, Abha 61421, Saudi Arabia;
sprakash@kku.edu.sa
4 Prosthetic Dental Science Department, Faculty of Dentistry, Najran University, P.O. Box 1988,
Najran 11001, Saudi Arabia
5 Department of Prosthodontics, Faculty of Stomatology, Yerevan State Medical University after Mkhitar
Heratsi, Str. Koryun 2, Yerevan 0025, Armenia; heboyan.artak@gmail.com
6 Department of Conservative Dentistry & Endodontics, Saveetha Dental College & Hospitals, Saveetha
Institute of Medical, Technical Sciences University, Chennai 600077, India; dr.isaq@gmail.com
7 Department of Restorative Dentistry & Endodontics, Faculty of Dentistry, University of Puthisastra,
Phnom Penh 12211, Cambodia
* Correspondence: nimishakakkad.nk@gmail.com (N.K.); aldowah@gmail.com (O.A.)
Abstract: This in vitro research aimed to evaluate the Tensile Bond Strength of Poly Ether Ether Ke-
tone and Zirconia copings using resin cement with or without Visio.link adhesive. From commercially
available Zirconia and PEEK, blocks were machined milled using (CAD)/(CAM) to obtain 20 Zirconia
and 20 PEEK copings. These specimens were sandblasted using 110 µm of alumina. The two main
groups (20 Zirconia and 20 PEEK copings) were divided further into 4 subgroups, GROUP 1 (n = 10)
PEEK substructure with self-adhesive resin cement without pretreatment, and GROUP 2 (n = 10)
PEEK substructure with self-adhesive resin cement pre-treated with Visio.link adhesive. GROUP 3
(n = 10) Zirconia copings with self-adhesive resin cement without pretreatment. GROUP 4 (n = 10)
Zirconia copings with self-adhesive resin cement pre-treated with Visio.link adhesive. Universal
testing machine was used to evaluate the tensile bond strength of these copings. The results were
analyzed using SPSS software Version 25.0 (SPSS Inc., Chicago, IL, USA). One-way ANOVA and
independent t-test were used to compare the mean scores. Statistically significant increase was
observed in Tensile Bond Strength of samples when Visio.link adhesive was used. Tensile Bond
Strength of PEEK copings and Zirconia copings with Visio.link adhesive is considerably greater than
PEEK copings and Zirconia copings without adhesive. The mean Tensile Bond Strength of Zirconia
(with or without adhesive) is less as compared to Tensile Bond Strength of PEEK (with or without
adhesive), but the difference is not statistically significant.
Keywords: PEEK; resin cement; tensile bond strength; visio.link adhesive; Zirconia
1. Introduction
PEEK (Poly Ether Ether Ketone), regarded as methacrylate-free semicrystalline ther-
moplastic material, is a crucial prototypical member of the polyacryletherketone (PAEK)
family [1]. It comprises aromatic benzene molecule along with functional ether or ke-
tone group. The earlier literature on PEEK has shown that it has better chemical, ther-
mal, mechanical, and biological properties in comparison to many restorative materials
https://www.mdpi.com/journal/materials
Materials 2022, 15, 4167 2 of 12

used today [2]. It eliminates the metallic taste and allergic reaction thus used for fabrica-
tion of metal framework in Removable Partial Denture, especially in patients allergic to
cobalt chromium framework. It is also used in the fabrication of provisional implant and
healing abutments [2,3].
PEEK is advantageous over other materials, however, its whitish color, low translu-
cency, and absence of durable bond limits its use as a restorative material [4]. Hence, to
overcome this limitation and enhance viscosity, bond durability and mechanical reten-
tion filler content of PEEK was increased [4,5]. The chemical adhesion is another way of
achieving durable bond. Studies have shown that, due to low surface energy of PEEK, the
bonding between the substructure and the resin cement decreased [4]. According to the
study done by Patrick R. Schmidlin, a failure rate of 15% was seen with copings aluminum
oxide sand blasted, but only when adhesive was not used [6].
Adhesives improve the bonding by complex exchange between the substructure and
resin cement [2]. Higher bond strength can be attained by adhesives with compositions of
Methylmethacrylate (MMA) and Dimethacrylate (DMAs) [7].
Zirconia, on the other hand, has proven chemical and dimensional stability. It has
opened new horizons for metal-free dentistry in the past few years. It has superior wear
resistance in comparison with other ceramic materials [8]. The most common problems
associated with zirconia restorations are chipping and debonding. Surface roughness and
the type of bonding agent used determine the binding strength of zirconia [9].
Visio.link is a light curing bonding agent (primer) for veneers and artificial teeth based
on polymethylmethacrylate and composites. It ensures firm bonding of highly cross-linked
PMMA teeth. Researchers have shown that visio.link has the highest bond strength with
PEEK restorations when used following ideal protocol and alumina blasting. Visio.link
is a bonding agent that incorporates methyl methacrylate monomer. As a result, it is
possible that the visio.link dissolved the tested PEEK material at its surface, and the free
carbon double bond polymerized with carbon compounds from the bonding agent and
the resin composite cement. MMA and PETIA (pentaerythritol triacrylate) are the two
primary components of Visio.link. Visio.link gave higher binding strength values to PEEK
restorations because of PETIA’s high capacity to change the PEEK surface [10].
Tensile Bond Strength helps us to determine the load at which the adhesive bond of
resin cement with coping and tooth fails and dislodgement of coping takes place.
The studies done before were on PEEK material to determine the best adhesive and
pre-treatment required to increase the bond strength and thus the durability of the restora-
tion. However, the most commonly used aesthetic material, along with PEEK, is Zirconia.
Previous studies have shown that applying a 10-Methacryloyloxydecyl dihydrogen phos-
phate (MDP)-containing bonding or silane-bonding agent mixture to ceramic zirconia
yields superior shear bond strength. In a study done by Hasan Sarfaraj et al. in 2020,
6-methacryloyloxyhexyl phosphonoacetate (6-MHPA) was used as an adhesive agent for
zirconia and composite veneer. The good chemical interaction between the 6-MHPA or
6-MHPP (-P(=O)(OH)2) phosphonic acid group and metal oxides on the zirconia surface
was assumed to be responsible for the effective zirconia bonding [11]. Previous research by
Bonga Stawarczy in 2013 found that increasing the surface area of PEEK using airborne-
particle abrasion and using MMA-containing adhesive solutions improves the bonding
characteristics [4]. In the present study, we will see the bond strength of zirconia with MMA
containing adhesive and the comparison of PEEK and Zirconia tensile bond strength.
The null hypothesis tested was that there are no differences in the Tensile Bond
Strength of Poly Ether Ether Ketone and Zirconia using resin cement with or without
Visio.link adhesive.

2. Materials and Methods

This experimental in vitro study aims to evaluate the Tensile Bond Strength of PEEK
and Zirconia copings on freshly extracted maxillary central incisor under universal testing
 machine beforecopings
and Zirconia the commencement of study
on freshly extracted IEC approval
maxillary was obtained
central incisor with re
under universa
number 2019/IEC/300/3.
machine before the commencement of study IEC approval was obtained with r
The inclusion
number criteria for the study was freshly extracted maxillary central
2019/IEC/300/3.
and exclusion criteria
The inclusion were for
criteria posterior tooth,
the study wascarious
freshlytooth, restored
extracted tooth,centra
maxillary or fra
Materials 2022, 15, 4167
tooth.
3 of 12
and exclusion criteria were posterior tooth, carious tooth, restored tooth, or f
tooth.
2.1. Fabrication of Specimen
machine before the commencement of study IEC approval was obtained with reference
2.1.A
number freshly
Fabrication extracted
of Specimen
2019/IEC/300/3. Maxillary Central Incisor was collected from Oral and Ma
cial Surgery
The department.
inclusion
A freshly
criteria
extracted
for Patient
the study consent
Maxillary was
was freshly
Central taken,maxillary
extracted patient was afrom
central knownOralcase
incisor, and
andofM
exclusion criteria were posterior tooth, carious tooth,Incisor
restoredwas collected
tooth, or fractured tooth.
sive
cialperiodontitis,
Surgery department. and extractionPatientofconsent
mobile was toothtaken,
was done.
patient The wascalculus
a known deposits
case oa
tissue
sive
2.1. debris were
periodontitis,
Fabrication washed
of Specimen off usingof0.5%
and extraction mobile sodium
toothhypochlorite
was done. The and tap water.
calculus The
deposits
teeth
tissue were
debris
A freshly used in the
were washed
extracted study
Maxillaryoff because
using
Central we
0.5%
Incisor needed
wassodium to
collected gauge
hypochloritethe bond
from Oral and and strength
tap water. Th
Maxillofacial of pe
zirconia adhesively
Surgery department.
teeth were used inluted to human
Patient consent
the study
was dentin.
because The tooth
taken, patient
we needed to was
was a known
gauge then
caseentrenched
of aggressiveinto a se
the bond strength of p
acrylic resin block. The tooth was prepared under standard
periodontitis, and extraction of mobile tooth was done. The calculus deposits and soft tissue
zirconia dimension for all c
debris wereadhesively
washed off using luted0.5%to human dentin. Theand
sodium hypochlorite tooth
tap was
water.then
The entrenched
natural teeth into a
crown,
acrylic
were usedand
resin
in thea shoulder
block.because
study The gingival
tooth finish
was
we needed line the
toprepared
gauge of 1bond
mmstrength
under width ofwas
standard uniformly
and zirconia made.
peekdimension for all
pression
crown, and a shoulder gingival finish line of 1 mm width was uniformly madeT
adhesively of prepared
luted to human tooth was
dentin. Themade
tooth using
was addition
then entrenchedpolyvinylsiloxane
into a self-cure material.
acrylic
pression
resin block.was
pression of then
tooth sent
Theprepared to a commercial
tooth
was prepared was made
under lab (Kolaj
using
standard Dental
addition
dimension Lab PUNE,
forpolyvinylsiloxane
all ceramic Pune,
crown, India)
material.
and
rication
a shoulder
pression ofwas PEEK
gingival
then and
finish
sent Zirconia
line of 1 mmcopings lab
to aaddition
width
commercial using
was CAD/CAM
uniformly
(Kolaj
made.
Dental The software
An
Lab PUNE,(Ceramill®E
impression of
Pune,
prepared tooth was made using polyvinylsiloxane material. impression was India
CAD,
rication
then
Kolaj
sent toof
Dental
PEEK and
a commercial
Lab, Pune,
lab Zirconia
India)
copings
(Kolaj Dental
(Figures
Lab PUNE, using 1–3). The
CAD/CAM
Pune,
lab was instructed
software
India) for fabrication
to cre
(Ceramill®
of PEEK
mmCAD,
and holeKolaj
Zirconiabuccolingually
Dental
copings Lab,
using below
Pune,the
CAD/CAM incisal
India)
software edge
(Figures in all the
1–3).
(Ceramill®EXO The copings
4.0 lab
CAD, was during fabricatio
instructed
Kolaj Dental to c
was done to facilitate the placement of a 23-gauge wire
mm hole buccolingually below the incisal edge in all the copings during fabricat
Lab, Pune, India) (Figures 1–3). The lab was instructed to create a 1 in
mm the
hole hole to provide
buccolingually anc
ofwas
the done
below copings
the incisal to the upper
edge
to facilitate
in all the cross head of
copings
the placement
during of auniversal
23-gaugetesting
fabrication.
wire inmachine
This was done
the hole(Figure
to facilitate the 4). an
to provide
placement of a 23-gauge wire in the hole to provide anchorage of the copings to the upper
of the
cross copings
head to the
of universal upper
testing cross(Figure
machine head of4). universal testing machine (Figure 4).

Figure 1. Fabrication of coping in CAD/CAM.

Figure
Figure 1. Fabrication
1. Fabrication of coping
of coping in CAD/CAM.
in CAD/CAM.

(A) (B)
Figure
Figure 2.2.(A)
(A)PEEK
PEEK (A)
coping,
coping, (B) Zirconia
(B) Zirconia coping. coping. (B)
Figure 2. (A) PEEK coping, (B) Zirconia coping.
Materials 2022, 15, x FOR PEER REVIEW
Materials 2022, 15, x FOR PEER REVIEW
Materials 2022, 15, 4167 4 of 12

Figure 3. Coping seated on the specimen.

Figure
Figure 3. 3. Coping
Coping seated
seated on theon the specimen.
specimen.

Figure
Figure 4. 4. 1 mm
1 mm holehole buccolingually
buccolingually below
below the incisalthe incisal
edge edge23-gauge
in coping, in coping,
wire 23-gauge wire passing
passing through
Figure 4. 1 mm hole buccolingually
the hole to provide anchorage.
the hole to provide anchorage. below the incisal edge in coping, 23-gauge wire passing
the hole to provide anchorage.
The specimens were surface treated using sandblasting of 110 µm of aluminum oxide.
TheThe specimens
sample were
consisted of 20surface
Zirconiatreated usingcopings.
and 20 PEEK sandblasting of 110size
This sample μm of alumi
was
The specimens were surface treated using sandblasting of 110 μm of alumi
ide. because it was the minimum required number to obtain statistically significant
selected
ide. These groups were further divided depending upon the use of adhesive. The groups
result. The sample consisted of 20 Zirconia and 20 PEEK copings. This sample size
The sample consisted of 20 Zirconia and 20 PEEK copings. This sample size
are as follows:
lected because it was the minimum required number to obtain statistically signif
lected because
Groups it Treatments
surface was the minimum required number to obtain statistically signif
sult. These groups were further divided depending upon the use of adhesive. The
1.sult.GROUP
These groups
1 (n = 10): were
PEEKfurther divided
substructure depending
cemented upon the use
with self-adhesive of cement
resin adhesive. The
are as follows:
are using
as follows:
no pre-treatment.
2. Groups2 (n
GROUP surface
= 10): Treatments
PEEK substructure cemented with self-adhesive resin cement
Groups surface Treatments
1. pre-treated
GROUP using 1 (n =visio.link
10): PEEK substructure cemented with self-adhesive resin cem
adhesive
3.1. GROUP
GROUP 1=(n = Zirconia
ing no pre-treatment.
3 (n 10): 10): PEEK substructure
copings cemented
cemented with withresin
self-adhesive self-adhesive
cement usingresin cem
ing no pre-treatment.
2. noGROUP 2 (n = 10): PEEK substructure cemented with self-adhesive resin cem
pre-treatment.
4.2. GROUP
GROUP 4 (n2 =(n10):
= 10): PEEK
Zirconia substructure
copings cementedcemented with self-adhesive
with self-adhesive resin cem
resin cement pre-
treated using visio.link adhesive
treated using visio.link adhesive
treated using visio.link adhesive.
3. GROUP 3 (n = 10): Zirconia copings cemented with self-adhesive resin ceme
3. Group
GROUP 1 (n =310):
(n = 10): Zirconia copings cemented with self-adhesive resin ceme
no pre-treatment.
no pre-treatment.
Resin cement (Rely X Luting2; 3M ESPE) was mixed and manipulated following
4. GROUPinstruction
manufacturer’s 4 (n = 10): andZirconia
the PEEKcopings cemented
copings were with
light cured forself-adhesive resin cem
5 s and cemented.
4. Group
GROUP 410):
(n = 10): Zirconia copings cemented with self-adhesive resin cem
treated using visio.link adhesive.
2 (n =
treated adhesive
using visio.link adhesive.
Group 1 (n = 10):
Visio.link was applied on the PEEK copings for 5 s using brush, then Vi-
sio.linkGroup 1 (n = 10):for 90 s with the help of halogen light curing unit (HAL-LCUs).
was polymerized
Resin cement (Rely X Luting2; 3M ESPE) was mixed and manipulated fo
Resin cement
The polymerization time(Rely X Luting2;
was chosen according 3M ESPE)
to the was mixed
manufacturer and manipulated
recommendation. Af- fo
manufacturer’s
ter the application of instruction and
adhesive, the thecement
resin PEEK(Relycopings were 3M
X Luting2; light cured
ESPE) wasfor 5 s and ce
mixed
manufacturer’s instruction and the PEEK copings were light cured for 5 s and ce
Group 2 (n
and manipulated = 10): to the manufacturer’s instruction and the PEEK copings were
according
Group 2 (nwas
= 10):
Visio.link adhesive
cemented. Cement wasfor
light cured applied on the PEEK copings for 5 s using brush,
5 s per side.
Visio.link adhesive was applied on the PEEK copings for 5 s using brush,
sio.link was polymerized for 90 s with the help of halogen light curing unit (HAL
sio.link was polymerized for 90 s with the help of halogen light curing unit (HAL
The polymerization time was chosen according to the manufacturer recommenda
The polymerization time was chosen according to the manufacturer recommenda
ter the application of adhesive, the resin cement (Rely X Luting2; 3M ESPE) wa
ter the application of adhesive, the resin cement (Rely X Luting2; 3M ESPE) wa
and manipulated according to the manufacturer’s instruction and the PEEK copin
 Materials 2022, 15, 4167 5 of 12

Materials 2022, 15, x FOR PEER REVIEW 5 of 12

Materials 2022, 15, x FOR PEER REVIEW 5 of 12
Group 3 (n = 10):
Resin cement (Rely X Luting2; 3M ESPE) was mixed and manipulated according to
Group 4 (n = instruction
the manufacturer’s 10): and the zirconia copings were cemented and light cured for
Group 4 (n = 10):
5 s perVisio.link
side. adhesive was applied on the Zirconia copings for 5 s using a brush, then
Visio.link adhesive was applied on the Zirconia copings for 5 s using a brush, then
Visio.link
Groupwas 4 (n polymerized
= 10): for 90 s with the help of HAL-LCUs. The polymerization time
Visio.link was adhesive
polymerized for 90 s with the help ofcopings
HAL-LCUs. for 5 The polymerization
a brush, thentime
was chosen according to
Visio.link wastheapplied
manufacturer’s
on the recommendation.
Zirconia s using
was chosen according to the manufacturer’s recommendation.
After
Visio.link wasthepolymerized
applicationfor of 90
adhesive,
s with the the resin
help cement (Rely
of HAL-LCUs. TheX polymerization
Luting2; 3M ESPE) time was
was After
chosen the application
according to the of adhesive,
manufacturer’s the resin cement (Rely X Luting2; 3M ESPE) was
recommendation.
mixed and manipulated according to the manufacturer’s instruction and the Zirconia cop-
mixed and manipulated
applicationaccording to the
the manufacturer’s instruction and theESPE)
Zirconia
was cop-
ingsAfter
werethecemented. of adhesive,
Cement was light resin cement (Rely
cured for 5 s per side. X Luting2; 3M
ings were
mixed andcemented.
manipulated Cement was light
according to thecured for 5 s per side.
manufacturer’s instruction and the Zirconia
copings were cemented. Cement was light cured for 5 s per side.
2.2. Testing of Specimen for Tensile Bond Strength
2.2. Testing of Specimen for Tensile Bond Strength
Universal
2.2. Testing Testing
of Specimen Machine
for Tensile Bond(UTM)
Strengthwas employed to evaluate the tensile bond
Universal Testing Machine (UTM) was employed to evaluate the tensile bond
strength of
Universal the samples. A 23-gauge wire was attached through the hole for testing the
strength of theTesting
samples.Machine (UTM) was
A 23-gauge wire employed
was attached to evaluate the tensile
through bond
the hole forstrength
testing the
specimens as shown in Figure 4. The machine consists of an
of the samples. A 23-gauge wire was attached through the hole for testing the specimens upper holding device
as and
specimens as shown in Figure 4. The machine consists of an upper holding device and
lower in
shown holding
Figuredevice. The acrylic
4. The machine resinofblock
consists was fixed
an upper holdingin device
lower holding
and lower device and the
holding
lower holding device. The acrylic resin block was fixed in lower holding device and the
loop wire
device. The attached to the
acrylic resin blockspecimen
was fixedwas engaged
in lower by upper
holding deviceholding
and the loopdevice.
wire attached
loop wire attached to the specimen was engaged by upper holding device.
to the The universal
specimen was testing
engagedmachine
by upper (INSTRON
holding device. 3382 series operating on Bluehill software)
Theuniversal
universaltesting
testingmachine
machine (INSTRON 3382 series operating on Bluehill software)
with a crosshead speed of 0.5 mm/min was3382
The (INSTRON usedseries
to dislodge
operating theoncemented
Bluehill copings and
software)
with a crosshead speed of 0.5 mm/min was used to dislodge the cemented
copings and the and
copings
the force
with required
a crosshead speedforof the
0.5same was measured
mm/min was used to(Figures
dislodge5the andcemented
6).
the force
force required
required for theforsame
the same was measured
was measured (Figures (Figures
5 and 6).5 and 6).

Figure 5. INSTRON 3382 series operating on Bluehill software Universal Testing Machine.
Figure5.5.INSTRON
Figure INSTRON3382
3382series
series operating
operating onon Bluehill
Bluehill software
software Universal
Universal Testing
Testing Machine.
Machine.

Figure6.6.Showing
Figure Showingthe
the specimen
specimen in in Universal
Universal Testing
Testing Machine.
Machine.
Figure 6. Showing the specimen in Universal Testing Machine.

The readings at which copings were debonded were noted (Figure 7). The dislodging
The readings at which copings were debonded were noted (Figure 7). The dislodging
force measured in Newton (N) was changed into MegaPascals (MPa) by dividing it with
force measured in Newton (N) was changed into MegaPascals (MPa) by dividing it with
the surface area (mm2) of the prepared tooth. The below-mentioned formula was used to
the surface area (mm2) of the prepared tooth. The below-mentioned formula was used to
calculate the surface area of tooth.
 Materials 2022, 15, 4167 6 of 12

Materials 2022, 15, x FOR PEER REVIEW The readings at which copings were debonded were noted (Figure 7). The dislodging 6 of 12
force measured in Newton (N) was changed into MegaPascals (MPa) by dividing it with
the surface area (mm2 ) of the prepared tooth. The below-mentioned formula was used to
calculate the surface area of tooth.
Area = π/4 d12 + πh/2 (d1 + d2) + π/4 (d32 − d22)
Area = π/4 d12 + πh/2 (d1 + d2) + π/4 (d32 − d22)
where d1—diameter at the top of the preparation, d2—diameter at the base of the prepa-
ration,
where d3—diameter
d1—diameter atofthe
thetop
base of the
of the preparation
preparation, plus 1 mm
d2—diameter at margins either
the base of side, h—
the preparation,
axial height.
d3—diameter of the base of the preparation plus 1 mm margins either side, h—axial height.

(A) (B)
Figure
Figure7.7.(A)
(A)Force
Forcewas
wasapplied
appliedtotodislodge
dislodgethe
thecemented
cementedcopings.
copings.(B)
(B)The
Thereadings
readingsatatwhich
whichcopings
copings
were debonded were noted.
were debonded were noted.

The
Thedimension
dimensionofofthe thetooth
toothwas
wasmeasured
measuredusing
usingVernier
VernierCalliper.
Calliper.The
Thefollowing
followingare
are
the
thespecification:
specification:
d1
d1==2 2mm
mm
d2
d2 = 4.7mm
= 4.7 mm
hh==7.5
7.5mmmm
d3
d3==5.7
5.7mmmm
Thus,
Thus,the
thesurface
surface area
area calculated was 90.232
calculated was 90.232 mm
mm22.. The
The following
followingformula
formulawaswasused
usedto
tomeasure
measurethethetensile
tensilebond
bondstrength:
strength:
Tensilebond
Tensile bondstrength
strength(Mpa)
(Mpa)= =Force
Force(N)
(N)××Area (mm22))
Area (mm

2.3.Statistical
2.3. StatisticalAnalysis
Analysis
Data was calculated in Microsoft Excel spreadsheet and descriptive data was evaluated
Data was calculated in Microsoft Excel spreadsheet and descriptive data was evalu-
using SPSS software Version 25.0 (SPSS Inc., Chicago, IL, USA). The statistical test one-way
ated using SPSS software Version 25.0 (SPSS Inc., Chicago, IL, USA). The statistical test
ANOVA and independent t-test were used to obtain the results.
one-way ANOVA and independent t-test were used to obtain the results.
3. Results
3. Results
The dependent variables used in the study were zirconia, PEEK (a high-performance
The dependent
polymer), variables
resin cement, used in the
and Visio.link study were zirconia, PEEK (a high-performance
adhesive.
polymer), resin cement, and Visio.link adhesive.
The outcome of the result depicted that the mean tensile bond strength of Poly Ether
The outcome
Ether Ketone of the
(PEEK) result depicted
without visio.linkthat the mean
adhesive tensile
group was bond
0.607 strength
+ 0.0211 of Polyand
(MPa) Ether
for
Ether Ketone (PEEK) without visio.link adhesive group was 0.607 + 0.0211 (MPa)
PEEK with visio.link adhesive group it was more 1.292 + 0.0282 (MPa), thus the result and for
PEEK
showswith visio.linkdifference
a significant adhesive between
group itthese
was more
groups1.292 + 0.0282
(p-0.000) (MPa),
(Figure thus 1).
8) (Table the result
shows a significant difference between these groups (p-0.000) (Figure 8) (Table 1).
 Materials 2022, 15, x FOR PEER REVIEW 7 of 12
Materials
Materials 2022, 15, 4167
2022, 15, x FOR PEER REVIEW 7 of 127 of 12

PEEK without or with visio.link adhesive

PEEK without or with visio.link adhesive

2
2

1
1
0.5 0.7 0.9 1.1 1.3
0.5 0.7 0.9Strength(MPa)1.1
Tensile Bond 1.3
Tensile Bond Strength(MPa)
Figure 8. Comparison of mean tensile bond strength of poly ether ether ketone (PEEK) with and
without visio.link adhesive. Vertical Axis: 1—PEEK without Visio.link adhesive, 2—PEEK with Vi-
Figure 8.Comparison
Comparison ofof mean tensile bond strength of poly
etherether
etherether ketone (PEEK) with and
sio.link8.adhesive.
Figure mean tensile bond strength of poly ketone (PEEK) with and
without visio.link adhesive. Vertical Axis: 1—PEEK without Visio.link adhesive,
without visio.link adhesive. Vertical Axis: 1—PEEK without Visio.link adhesive, 2—PEEK with2—PEEK with Vi-
sio.link adhesive.
Table 1. Particulars
Visio.link adhesive. for mean tensile bond strength of PEEK with and without visio.link adhesive.

Table
Table 1. 1.
Particulars forPEEK
Particulars for
mean without
mean tensile
tensile bondVisio.Link
bond strength
strength Adhe-
of PEEK
of PEEK PEEK
withwith with
and Visio.Link
without
and without Adhe-
visio.link
visio.link adhesive.
adhesive.
Particulars
sive sive Adhesive
Particulars PEEK without
PEEK without Visio.Link
Visio.Link Adhe-
Adhesive PEEK
PEEK withwith Visio.Link Adhe-
Visio.Link
Particulars
Minimum 0.57 1.24
Minimum sive
0.57 1.24 sive
Quartile
Quartile 11 0.59
0.59 1.27
1.27
Minimum
Median 0.57
0.61 1.301.24
Median 0.61 1.30
Quartile
Quartile 331
Quartile 0.59
0.62
0.62 1.311.27
1.31
Median
Maximum
Maximum 0.61
0.63
0.63 1.321.30
1.32
Quartile 3 0.62 1.31
Maximum
Themean
The meantensile
tensilebond
bondstrength 0.63
strengthofofZirconia
Zirconiawithout
withoutvisio.link 1.32group
visio.linkadhesive
adhesive groupwas
was
0.549++0.0375
0.549 0.0375 (MPa)
(MPa) andandforforZirconia with
Zirconia visio.link
with adhesive
visio.link group
adhesive it wasitmore
group was 1.225
more+
0.0317
1.225 (MPa)
+The
0.0317 andtensile
mean
(MPa) theand
difference
bond betweenbetween
strength
the difference ofthe groups
Zirconia was alsowas
the without
groups highly
alsosignificant
visio.link adhesive
highly (p-0.000)
group was
significant
(Figure
0.549 + 9)
(p-0.000) (Table
0.0375
(Figure 9)2).
(MPa) and
(Table 2).for Zirconia with visio.link adhesive group it was more 1.225 +
0.0317 (MPa) and the difference between the groups was also highly significant (p-0.000)
(Figure 9) (Table 2). Zirconia without or with visio.link adhesive

Zirconia without or with visio.link adhesive

2

1
0.3 0.5 0.7 0.9 1.1 1.3
Tensile Bond Strength(MPa)

Figure9.9.Comparison
Figure Comparisonof
of0.3
meantensile
mean tensile
0.5bondstrength
bond strength
0.7 ofofZirconia
Zirconia withand
0.9with and1.1
withoutvisio.link
without visio.link adhe-
1.3 adhe-
sive.VerticalAxis:1—Zirconia
sive.Vertical Axis:1—Zirconiawithout
withoutVisio.link
Visio.linkadhesive,
adhesive,2—Zirconia
2—Zirconiawith
withVisio.link
Visio.link adhesive.
adhesive.
Tensile Bond Strength(MPa)

Figure 9. Comparison of mean tensile bond strength of Zirconia with and without visio.link adhe-
sive.Vertical Axis:1—Zirconia without Visio.link adhesive, 2—Zirconia with Visio.link adhesive.
 Materials 2022, 15, x FOR PEER REVIEW 8 of 12

Materials 2022, 15, 4167 8 of 12

Table 2. Particulars for mean tensile bond strength of Zirconia with and without visio.link adhe-
sive.
Table 2. ParticularsZirconia without
for mean tensile bondVisio.Link Ad- Zirconia
strength of Zirconia with Visio.Link
with and without Ad-
visio.link adhesive.
Particulars
Particulars Zirconia withouthesive
Visio.Link Adhesive hesive Adhesive
Zirconia with Visio.Link
Minimum
Minimum 0.49
0.49 1.19
1.19
Quartile11
Quartile 0.5225
0.5225 1.2025
1.2025
Median
Median 0.55
0.55 1.215
1.215
Quartile33
Quartile 0.575
0.575 1.24
1.24
Maximum 0.61 1.28
Maximum 0.61 1.28

Thecomparative
The comparativedifference
difference in Tensile
in Tensile BondBond Strength
Strength between between
Zirconia Zirconia and
and PEEK-
PEEKgroup was Zirconia without visio.link adhesive showed 0.549 + 0.0375 and
group was Zirconia without visio.link adhesive showed 0.549 + 0.0375 (MPa) (MPa) and
mean
mean tensile
tensile bond strength
bond strength of PolyofEther
Poly Ether
Ether Ketone
Ether Ketone
(PEEK) (PEEK)
withoutwithout visio.link
visio.link adhesive
adhesive was
was 0.607+
0.607 0.0211
+ 0.0211 (MPa).
(MPa). For For
PEEKPEEKwithwith visio.link
visio.link adhesive
adhesive waswas 1.292
1.292 + +0.0282
0.0282(MPa),
(MPa),and
and
for Zirconia with visio.link adhesive was 1.225 + 0.0317 (MPa). Both the
for Zirconia with visio.link adhesive was 1.225 + 0.0317 (MPa). Both the groups with vi- groups with
visio.link adhesiveshowed
sio.link adhesive showedmoremore mean
mean tensile
tensile bond
bond strength
strength compared
compared to to those
thosewithout
without
visio.link
visio.link adhesive group, and the result showed a significant difference betweenthese
adhesive group, and the result showed a significant difference between these
groups
groups(p-0.000)
(p-0.000)(Figure
(Figure10)
10)(Table
(Table3).3).

Zirconia and PEEK with or without visio.link adhesive

0.4 0.6 0.8 1 1.2 1.4 1.6

Tensile Bond Strength(MPa)

Figure10.
Figure 10. comparison
Comparisonof of
mean tensile
mean bond
tensile strength
bond of poly
strength of ether
poly ether
ether ketone (PEEK) (PEEK)
ether ketone and Zirconia
and
with and without visio.link adhesive.Vertical Axis: 1—Zirconia without Visio.link adhesive,
Zirconia with and without visio.link adhesive.Vertical Axis: 1—Zirconia without Visio.link 2—Zir-
ad-
conia with Visio.link adhesive, 3—PEEK without Visio.link adhesive, 4—PEEK with Visio.link ad-
hesive, 2—Zirconia with Visio.link adhesive, 3—PEEK without Visio.link adhesive, 4—PEEK with
hesive.
Visio.link adhesive.
Table3.3.Particulars
Table Particularsofofmean
meantensile
tensilebond
bondstrength
strengthofofpoly
polyether
etherether
etherketone
ketone(PEEK)
(PEEK)and
andZirconia
Zirconia
with and without visio.link adhesive.
with and without visio.link adhesive.
Zirconia without Zirconia with PEEK without Vi- PEEK with Vi-
Particu-
Zirconia without Zirconia with Visio.Link PEEK without PEEK with Visio.Link
Particulars Visio.Link Adhe- Visio.Link
Visio.Link sio.Link
Adhesive Adhe- Adhesive
sio.Link Adhe-
lars
Visio.Link Adhesive Adhesive
Minimum 0.49 sive 1.19 Adhesive 0.57 sive 1.24sive
Quartile 1 Minimum
0.5225 0.491.2025 1.19 0.5925 0.57 1.27251.24
Median Quartile 1
0.55 0.52251.215 1.2025 0.615 0.5925 1.31.2725
Quartile 3 0.575
Median 0.55 1.24 1.215 0.62
0.615 1.3175
1.3
Maximum 0.61 1.28 0.63 1.32
Materials 2022, 15, x FOR PEER REVIEW 9 of 12

Materials 2022, 15, 4167 9 of 12

Quartile 3 0.575 1.24 0.62 1.3175
Maximum 0.61 1.28 0.63 1.32

When we
When we compare
compare the the PEEK
PEEK (with
(with and
and without
without visio.link
visio.link adhesive)
adhesive) and
and zirconia
zirconia
(with and without visio.link adhesive) groups, the mean tensile bond strength of Zirconia
(with and without visio.link adhesive) groups, the mean tensile bond strength of Zirconia
was
wasless
less0.0.887
887++ 0.3484
0.3484 compared
compared to
to PEEK
PEEK group
group0.949
0.949++ 0.3522,
0.3522, but
but the
the result
resultshows
showsnono
statistically significant difference (p-0.576) (Figure 11) (Table 4).
statistically significant difference (p-0.576) (Figure 11) (Table 4).

Comparison of mean tensile bond strength of

polyetheretherketone(PEEK) and Zirconia

0.3 0.5 0.7 0.9 1.1 1.3 1.5

Tensile Bond Strength(MPa)

Figure11.
Figure 11. Comparison
Comparison of
of mean
mean tensile
tensile bond
bondstrength
strengthof
ofpoly
polyether
etherether
etherketone
ketone(PEEK)
(PEEK)and Zirco-
and Zir-
nia.Vertical Axis: 1—Zirconia with without Visio.link adhesive, 2—PEEK with and without Vi-
conia.Vertical Axis: 1—Zirconia with and without Visio.link adhesive, 2—PEEK with and without
sio.link adhesive.
Visio.link adhesive.
Table 4. Particulars of mean tensile bond strength of poly ether ether ketone (PEEK) and Zirconia.
Table 4. Particulars of mean tensile bond strength of poly ether ether ketone (PEEK) and Zirconia.
Zirconia with without Visio.Link PEEK with and without Vi-
Particulars Zirconia with and without PEEK with and without
Particulars Adhesive
Visio.Link Adhesive sio.Link
Visio.LinkAdhesive
Adhesive
Minimum
Minimum 0.49
0.49 0.57
0.57
Quartile
Quartile11 0.55
0.55 0.6175
0.6175
Median
Median 0.90.9 0.935
0.935
Quartile 33
Quartile 1.2125
1.2125 1.3
1.3
Maximum 1.28 1.32
Maximum 1.28 1.32

Theobtained
The obtained mean
mean scores
scores were
wereanalyzed
analyzed using
using One-way
One-way ANOVA
ANOVAand andIndependent
Independent
t-test. In all the statistical analysis purposes, significant p-value was taken≤
t-test. In all the statistical analysis purposes, significant p-value was taken ≤0.05.
0.05.

4. Discussion
4. Discussion
Owing to increasing demand of aesthetically pleasing dental material, PEEK and
Owing to increasing demand of aesthetically pleasing dental material, PEEK and Zir-
Zirconia are the popularly used restorative materials. However, the major shortcoming of
conia are the popularly used restorative materials. However, the major shortcoming of
PEEK and Zirconia is the absence of durable bond, which must be achieved for long term
PEEK and Zirconia is the absence of durable bond, which must be achieved for long term
stability. The reasons for the absence of durable bond could be inadequate preparation
stability. The reasons for the absence of durable bond could be inadequate preparation of
of abutment teeth or wrong application technique, but the major reason is absence of
bonding agent [12]. Durable bond can be achieved by increasing mechanical retention or
by additional chemical adhesion. In this study, pretreatment with 110 µm aluminum oxide
particle was done to create roughness on copings surfaces, and thus increase mechanical
Materials 2022, 15, 4167 10 of 12

retention. A study done by Hiroyasu Koizumi et al. states that no effect of surfaces
pre-treatment alone can be seen on tensile bond strength of PEEK and Zirconia copings,
although use of visio.link adhesive increases the tensile bond strength significantly [13].
Chemical treatment following alumina abrasion significantly improves the bond strength
in comparison to chemical treatment without alumina abrasion [14]. The main explanation
for increasing the tensile bond strength after air abrasion is roughness that cannot be
created by chemical treatment only. The alumina abrasion increases the surface area, which
helps to increase the bond strength between two polymers [5]. Secondly, there will be
more functional groups by increasing the surface area, so therefore greater crosslinking of
polymer [5]. Kern and Lehmann in 2012 studied the bond strength of PEEK and provisional
resin using different methods of surface modifications and adhesive system for conditioning.
Mean tensile bond strength of 23.2 Mpa with visio.link adhesive and 7.4 MPa without
visio.link adhesive when sulfuric acid was taken as pretreatment of PEEK specimen This
study results showed the highest values of MMA-containing adhesive systems [15].
The study conducted by Wolfart et al. in 2019 also showed that air abrasion with
110 µm Al2 O3 activated the zirconia surface by increasing the roughness. The tensile
bond strength of Zirconia with air abrasion shows a value of 2.71 ± 0.478, whereas when
specimen were treated with HF acid they showed a tensile bond strength of 1.41 ± 0.338,
and the third group surface treated with Al2 O3 particles followed by 30 µm silica coated
Al2 O3 particles showed the value 4.22 ± 0.698. They concluded that air abrasion of the
copings and META containing adhesive resin shows an increase in bond strength [16].
Visio.link is made up of MMA (Methyl methacrylate), PETIA (Pentacrythritoltriacrylate),
dimethacrylate, and photoinitiator. One of the important factors responsible for increased
bond strength between PEEK and veneering resin is MMA monomers [11]. This was also
supported by the study of Kern and Lehmann in 2012, in which they concluded that a
satisfactory bond with resin varnish was achievable when the surfaces to be cemented were
air abraded. Tensile bond strength value 69.0 MPa was calculated when visio.link adhesive
was used for PEEK material, which is quite high in comparison with the other adhesives
used such as Z-Prime Plus, Ambarino P60, Monobond Plus, and Signum PEEK Bond
I+II [17]. Another contributory factor in favor of visio.link, which significantly enhances
the bond strength, is the presence of PETIA which highly modifies the PEEK structure [15].
For polymerization of Visio.link adhesive system different light curing units (LCUs) can be
used, such as Halogen light curing unit (HAL-LCU) or LED light curing unit for chair side
or lab side, respectively. Earlier research shows that PEEK copings cured using halogen
light curing unit had higher tensile bond strength than those cured by LED light curing
unit. It is basically due to the chemical composition of visio.link photo initiator diphenyl
trimethyl benzoyl phosphine oxide requiring certain wavelengths to cure successfully. It
shows maximum absorption at 380 nm, and the mentioned wavelength is provided mainly
by halogen LCU [18]. In this study, the adhesive visio.link was polymerized using halogen
LCU for 90 s to attain durable bonding.
Relyx luting 2 was resin modified with light cure options that shorten cleanup to sec-
onds. This cement was primarily used for Zirconia crowns, metal, and pediatric crowns [19].
For application, mix the paste for 20 s until evenly mixed. The cementation of the prosthesis
was done following the guidelines of the manufacturer.
Each specimen was subjected to a debonding force which was recorded using Univer-
sal Testing Machine.
The obtained results showed that mean Tensile bond strength of Poly Ether Ether
Ketone (PEEK) and Zirconia without visio.link adhesive group was 0.607 + 0.0211 and
0.549 + 0.0375 (MPa), respectively, and for PEEK and Zirconia with visio.link adhesive
group was 1.292 + 0.0282 and 1.225 + 0.0317 (MPa), respectively. Both the study groups
which used visio.link showed statistically highly significant bond strength (p-0.000).
Therefore, we can conclude that after application of adhesive the bond strength
of respective copings almost doubles. Therefore, the null hypothesis that there are no
Materials 2022, 15, 4167 11 of 12

differences in the Tensile Bond Strength of Poly Ether Ether Ketone, and Zirconia using
resin cement with or without Visio.link adhesive is rejected.
When we compare the PEEK (with and without visio.link adhesive) and zirconia
(with and without visio.link adhesive) groups, though the mean tensile bond strength of
Zirconia was less 0.887 + 0.3484 compared to PEEK group 0.949 + 03522, the results were
not statistically significant (p-0.576).
In this article, the tensile bond strength was measured in vitro without thermocycling,
and studies should be done after thermocycling for better evaluation of bond strength,
although the appropriate and adequate measures were used to control the technicality in
the specimen fabrication and to minimize errors while testing.
Future studies should be done to incorporate the composition of Visio.link adhesive to
resin cement for better clinical results.

5. Clinical Significance
Adhesive helps to build a durable bond of copings with resin cement. The use of
resin cement alone is not recommended. In clinical practice we have to include the use of
adhesive, and the results will be favorable.

6. Conclusions
Bonding of PEEK and Zirconia copings almost doubles after the use of Visio.link
adhesive. Adhesives increase the surface area and thus the bonding of copings with
natural tooth. Tensile bond strength of PEEK is more than Zirconia, but the difference is
not significant.

Author Contributions: Conceptualization, N.S.Y. and P.H.; methodology, N.K.; software, N.K.;
validation, N.S.Y., P.H. and K.S.; formal analysis, N.K. and M.I.K.; investigation, N.K.; resources,
S.B., V.V. and S.A.; data curation, S.N.; writing—original draft preparation, N.K., M.I.K. and O.A.;
writing—review and editing, P.H., S.A., O.A., A.H. and M.I.K.; visualization, V.V.; supervision, N.K.,
N.S.Y., O.A. and M.I.K.; project administration, O.A. and A.H. All authors have read and agreed to
the published version of the manuscript.
Funding: This research received no external funding.
Institutional Review Board Statement: The study was conducted in accordance with the Declaration
of Helsinki and approved by the Ethics Committee of Peoples Dental Academy, Peoples University,
Bhopal, with reference number 2019/IEC/300/3.
Informed Consent Statement: Not applicable.
Data Availability Statement: The data will be shared upon a reasonable request to the
corresponding author.
Acknowledgments: This research was supported by the Deanship of scientific research at King
Khalid University, Abha for their support through Short Research Project (RGP. 1/347/43) and Taif
University Researchers support project Number (TURSP-2020/62), Taif University, P.O. Box-11099,
Taif-21944, Saudi Arabia.
Conflicts of Interest: The authors declare no conflict of interest.

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