d e n t a l m a t e r i a l s 3 7 ( 2 0 2 1 ) 464–476

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Optimizing the fitting-surface preparation of

zirconia restorations for bonding to dentin

Alexander Franz a , Olivia Winkler a , Stefan Lettner a , Simon Öppinger a ,

Anna Hauser a , Marwan Haidar a , Andreas Moritz a , David C. Watts b ,
Andreas Schedle a,∗
a University Clinic of Dentistry, Medical University of Vienna, Austria
b School of Medical Sciences and Photon Science Institute, University of Manchester, Manchester, UK

a r t i c l e i n f o a b s t r a c t

Article history: Objectives. The aim of this study was to identify the relative strengths and weaknesses of
Accepted 7 December 2020 different interfaces within the multilayer structure of a zirconia crown restoration when
applying different surface pretreatments. These include the influence on shear strengths
of different air abrasion protocols, glaze-on techniques, zirconia primers and self-adhesive
Keywords: cements for either the complex structure: zirconia / self adhesive resin composite cement
Zirconia restorations (RCC) / bovine dentin substrate (part 1) or the RCC / zirconia substrate (part 2).
Adhesive cementation Methods. In Part 1, zirconia discs, pretreated by either glaze-on techniques or air abrasion
Zirconia-cement-interface using RocatecTM Soft, were bonded to bovine dentin substrates with different self-adhesive
Glaze-on-technique RCCs. In Part 2, steel-cylinders were bonded to zirconia cuboid substrates, pretreated by
Air abrasion either different protocols for air-abrasion or a glaze-on-technique, with different self-
adhesive RCCs. Shear bond strengths (SBS) were measured for all interfacial combinations.
Results. In part 1, application of air abrasion using RocatecTM Soft significantly increased
the SBS of zirconia to dentin compared to control specimens without pretreatment, while
glaze-on techniques did not increase the SBS. Pretreatment of zirconia surfaces with two
primers (either Clearfil Ceramic Primer, or Monobond S) showed significantly higher SBS
than the controls. Cementations with RelyX Unicem 2 Automix showed significantly higher
SBS than with MaxCem Elite. In Part 2, all air abrasion protocols increased the SBS, but there
was no significant difference between these protocols. Again the glaze-on technique did
not increase SBS. A significant difference between the two RCCs was again observed. When
zirconia substrates were air abraded, regardless of which protocol was applied, the highest
SBS were obtained by Calibra with P&B active followed by Panavia with or without Clearfil
Ceramic Primer Plus. Calibra applied without P&B active exhibited the lowest SBS.
Significance. Pretreatment of zirconia substrates using air abrasion and/or ceramic primers
increased the SBS of the zirconia cement interface. For all tested glaze-on treatments, in our
experimental setting no effect was observed.
© 2021 The Academy of Dental Materials. Published by Elsevier Inc. This is an open access
article under the CC BY license (http://creativecommons.org/licenses/by/4.0/).

∗
Corresponding author.
E-mail address: andreas.schedle@meduniwien.ac.at (A. Schedle).
https://doi.org/10.1016/j.dental.2020.12.001
0109-5641/© 2021 The Academy of Dental Materials. Published by Elsevier Inc. This is an open access article under the CC BY license
(http://creativecommons.org/licenses/by/4.0/).
 d e n t a l m a t e r i a l s 3 7 ( 2 0 2 1 ) 464–476
1. Introduction
Over the last 20 years, material-related advances have led to
a significant increase in the use of all-ceramic restorations.
These improvements are in biocompatibility, mechanical
properties and aesthetics. The procedure for cementation of
glass-ceramics has become standardized, involving: (i) etch-
ing the restoration with HF, then (ii) silanization to ensure
a durable bond between restoration and composite cement
via chemical and micromechanical mechanisms. However, in
contrast to glass ceramics, there is no uniform “gold standard”
for cementation of oxide ceramics such as zirconium oxide,
for which zinc phosphate, glass ionomer and self-adhesive
composite cements can be used. But these lack the advanta-
geous properties (increased fracture resistance and improved
retention) of composite cements which adhere to etched and
silanized glass ceramics [1].
This leads to low retention between zirconia restorations,
luting cement and tooth structure. Since zirconia does not
contain silicates, it is neither etchable nor can an effective
bond be achieved with silanes between restoration and luting
cement [2,3]. This means that conventional luting protocols
of glass ceramics cannot be applied to oxide ceramics [4].
Another problem is the low wettability of the zirconia surface,
which is hydrophobic [5]. However, successful cementation of
oxide ceramic restorations is an important factor for long-
term clinical success [3,4,6]. But stronger micromechanical
retention can be achieved via a rougher, larger or more ener-
getic surface that changes the wetting capacity and facilitates
the flow of cement into the roughened surface [7]. There have
been many attempts over the last 2 decades to increase the
roughness of zirconia surface to improve cement bonding
[2,4]. Proposed methods include grit blasting with different
materials and grain sizes, so-called “tribochemical coating”,
laser treatments [4], grinding, primer and acid treatment [3,7],
“plasma spraying” or silanization [1]. Alternative strategies
include establishing a glass layer on the zirconia surface,
known as “Internal Coating”, “Selective Infiltration Etching”
or “Glaze-on Techniques” [2,7–9]. Whereas, in “Selective Infil-
tration Etching”, a thin glass layer is applied to the surface
by means of a conditioning agent and then completely dis-
solved [2], in the “Internal Coating” and “Glaze-on” technique
the glass or porcelain layer is preserved as the “inner lining”
of the restoration. In the latter two methods [7,9] HF is applied
to the fired glass layer of the oxide ceramics to roughen the
surface. The silicates contained in the glass layer enable bond-
ing with silanes. The aforementioned “glaze-onẗechnique has
led to significantly increased bonding in some studies, which
were also considered in some systematic reviews and meta-
analyses [3,7,10]. In the “glaze-on” studies examined in these
reviews this technique was only tested in combination with
metals or composites, but not with dentin.
Another possibility for surface treatment is air abrasion
(grit blasting) with small particles of silica (SiO2 ) and/or
alumina (Al2 O3 ) particles. Specifically in the RocatecTM ,
RocatecTM Plus and RocatecTM Soft systems (3M), particles
of aluminium oxide with a silica coating are blasted at high
speed onto a ceramic workpiece. According to the manufac-
turer during this process components of the particles melt on
465
the ceramic surface and microdefects are created, resulting
in surface enlargement. The extent of these surface changes
depends on particle size, jet pressure, angle of incidence,
duration and working distance [11–13]. Multiple studies have
established the value of grit blasting [4,14]. Largely unexplored
- or insufficiently well documented - are comparisons of dif-
ferent grit blasting protocols with regard to the resultant bond
strength. Likewise, the combined effect of grit blasting grain
size and pressure is still largely unexplored. Furthermore,
there is insufficient data on whether primer addition can fur-
ther improve the SBS.
In order to achieve the aim of this study, to optimize the
fitting surface preparation of zirconia restorations for bonding
to dentin, the following objectives were investigated:
Part 1:
a) Coating of zirconia with glass ceramic using Zenostar
Magic Glaze Spray (ZM), IPS e.max Ceram Glaze Spray (IPS)
or Hotbond zirconnect Spray (HB) followed by etching with
HF and silanization.
b) Pretreatment of zirconia with RocatecTM Soft followed by
the application of a ceramic primer versus an universal
primer.
Both issues were investigated using zirconia discs bonded
via RCC to bovine dentin substrates.
Part 2:
a) Coating of zirconia with glass ceramic (HB) followed by
etching with HF and silanization.
b) Pretreatment of zirconia substrates with air abrasion using
different protocols followed by application of two universal
primers with and without MDP monomer and two RCCs
with and without MDP.
Both issues were investigated using stainless steel discs
bonded via RCC to zirconia substrates. The logic of using stain-
less steel (SS) discs is that adhesive failure will occur between
RCC/zirconia, rather than at the SS/RCC interface.
The following null-hypotheses were formulated:
(i) Coating of zirconia surfaces with glass-ceramic does not
improve bonding of composite cements to zirconia com-
pared to the control (untreated zirconia surfaces).
(ii) Air abrasion of zirconia surfaces does not increase bond-
ing via composite cements, regardless of grain size and
pressure.
(iii) Primers do not increase the bonding of composite
cements to zirconia.
(iv) Self-adhesive RCCs, with or without MDP, do not show
similar bond strenths for the bovine dentin/RCC/zirconia
interfaces (part 1) versus the RCC/zirconia interface (part
2).
2. Materials and methods
Materials are listed in Tables 1A, 1B, 1C. Study variables are
presented in Tables 2A, 2B and Fig. 1A, 1B.
466 d e n t a l m a t e r i a l s 3 7 ( 2 0 2 1 ) 464–476

Table 1A – Surface glazing agents.

Glaze Code Material Manufacturer Lot Numbers Formulation
HB DCMhotbond Dental Creativ Management 13-04-16 SiO2 , Al2 O3 , K2 O, Na2 O,
zirconnect spray GmbH, Rostock, Germany CaO, B2 O3
ZM Zenostar Magic Wieland Dental + Technik 3/11 ZrO2 ,HfO2 ,Y2 O3 ,Al2 O3 ,other
Glaze Spray GmbH & Co. KG, Pforzheim, oxides ≤ 1.0 %
Germany
IPS IPS e.max Ceram Ivoclar Vivadent, Schaan, U42646 SiO2 , Al2 O3 , ZnO, Na2 O,
Glaze Spray Liechtenstein K2 O, ZrO2 , CaO and P2 O5
propellent, isobutane

Table 1B – Surface etching/priming/bonding.

Function Code Material Manufacturer Lot Numbers Formulation
®
Etching HF Hydrofluoric acid Ultradent Porcelain BDVSC Buffered gelled hydrofluoric acid
9% Etch, Ultradent
Products GmbH,
Köln, Germany

Silane CS Calibra Silane Dentsply Sirona, 170124 Ethyl alcohol, acetone, water
Coupling Agent Bensheim, Germany

Bonding CUBQ Clearfill Kuraray Noritake 1H0018 10-Methacryloyloxydecyl dihydrogenphosphate

Universal Bond Dental Inc., Tokyo, (MDP), BisphenolA diglycidylmethacrylate,
Quick Japan 2-Hydroxyethylmethacrylate (HEMA),
hydrophilic amide monomers, colloidal silica,
silan coupling agent, sodium fluoride,
dl-Camphorquinon, ethanol, water,k-Etchant,
phosphoric acid, water, colloidal silica, pigment

MBP Monobond-Plus Ivoclar Vivadent, V30663 10-Methacryloyloxydecyl dihydrogen phosphate,

Schaan, Methacrylated phosphoric acid ester, adhesive
Primer
Liechtenstein monomers, ethanol
CCP Clearfil Ceramic 3M ESPE, Seefeld, 650011 10-Methacryloyloxydecyl dihydrogen phosphate,
Primer Germany 3-trimethoxysilylpropyl (3-MPS) methacrylate,
sulphide methacrylates ethanol
CCPP Clearfill Ceramic Kuraray Noritake 3L0025 3-Methacryloxypropyl trimethoxysilane,
Primer Plus Dental Inc., Tokyo, 10-Methacryloyloxydecyl dihydrogenphosphate,
Japan Ethanol
PBA Prime & Bond Dentsply Sirona, 1706000937 Phosphoric acid modified acrylate resin,
active Bensheim, Germany multifunctional Acrylate, bifunctional acrylate,
acidic acrylate, isopropanol, water, initiator,
stabilizer

Table 1C – Cementation with RCCs.

RCC Material Manufacturer Lot Number Formulation
Code
RXU RelyXTM Unicem 3M ESPE, Seefeld, 670242 Methacrylate monomers containing phosphoric acid groups,
2 Automix Germany Methacrylate monomers, Alkaline (basic) fillers, silanated
fillers, Initiator components, Stabilizers, Rheological additives,
Pigments
MCE Maxcem EliteTM Kerr Dental, 5495743 1,6-hexanediyl bismethacrylate, 2-hydroxy-1,3-propanediyl
Orange, USA bismethacrylate, 7,7,9(or 7,9,9)-trimethyl-4,13-dioxo-3,14-
dioxa5,12-diazahexadecane-1,16-diyl bismethacrylate,
3-trimethoxysilylpropyl methacrylate, 1,1,3,3-tetramethylbutyl
hydroperoxide
PSA PanaviaTM SA Kuraray Noritake 2A0218 Paste A:10-Methacryloyloxydecyl dihydrogen phosphate,
Cement Plus Dental Inc., bisphenol A diglycidylmethacrylate, triethyleneglycol
Automix Tokyo, Japan dimethacrylate (TEGDMA), hydrophobic aromatic
dimethacrylate, 2-Hydroxyethylmethacrylate, silanated
barium glass filter, silanated colloidal silica,
dl-Camphorquinone, peroxide, catalysts, pigments
CAU Calibra Universal Dentsply Sirona, 170222 Urethane Dimethacrylate, Di-and Tri-Methacrylate resins,
Bensheim, phosphoric acid, modified acrylate resin, Barium Boron Flouro
Germany Alumino Silicate Glass, organic peroxide Initiator,
camphorquinone, phosphene oxide, accelerators, butylated
hydroxy toluene,UV stabilizer, titaniumdioxide, iron oxide,
hydrophobic amorphous silicon dioxide
 d e n t a l m a t e r i a l s 3 7 ( 2 0 2 1 ) 464–476 467

Table 2A – Surface preparation of zirconia substrates and cementation.

Part 1 Part 2
®
Zirconia cylinders or 480 cylinders of Prettau Zirconia 480 cuboids of Y-TZP Cercon ht®
zirconia cuboids (6 mm diameter / 3 mm height). (12 mm edge length / 2 mm thickness)

Glazing Air abrasion Glazing Air abrasion

Air abrasion Pure Al2 O3 : Rocatec SOFT Pure Al2 O3 : Pure Al2 O3 :
Particle size 110 ␮m (R-TEC): Particle size 110 ␮m Group 1: Particle size 110
Pressure 2 bar Particle size 30 ␮m Pressure 2 bar ␮m, pressure 3.5 bar
Duration 15 s Pressure 2 bar Duration 5 sec Group 2: Particle size 110
Distance 10 mm Duration 15 s Distance 10 mm, ␮m, pressure 2 bar
Distance 10 mm Angle 45◦ Group 3: Particle size 50
␮m, pressure 2 bar
Group 4: Particle size 50
␮m, pressure 0.5 bar
For all four subgroups:
Distance 10 mm, angle 45◦ ,
duration 5−7 sec

Glazing HB, ZM or IPS: HB:

Sprayed in circular movement, Distance 10 cm
angle 90◦ , distance 10 cm

Air abrasion after HB and ZM: Pure Al2 O3

glazing Pure Al2 O3 Particle size 110 ␮m,
Particle size 110 ␮m Pressure 0.1 MPa
Pressure 1 bar Distance 10 mm
Duration 5 s. Angle 45◦
Distance 10 mm
IPS:
Pure Al2 O3,
Particle size 50 ␮m
Pressure 0.75 bar
Duration 5 s.
Distance 10 mm

HF-Treatment Hydrofluoric acid 9% Hydrofluoric acid 10%

60 s, rinsed for 30 s 60 s, rinsed for 60 s

Silanization/Priming Monobond Plus or Monobond Plus or Calibra Silane 60s P&B active or
Clearfill Ceramic Primer Clearfill Ceramic or Clearfil CCP plus
60 s Primer 60 s Clearfil CCP plus 60 s 20 s
For half of the specimens

Bonding P&B active or

Clearfil universal bond
for half of the
specimens

Self-adhesive Maxcem Elite or Maxcem Elite or Calibra Universal or Calibra Universal or

composite RelyX Unicem 2 Automix RelyX Unicem 2 Panavia SA Cement Plus Panavia SA Cement Plus
cements Automix

2.1. Part 1: Shear bond strength of zirconia cylinders

Table 2B – Pretreatment of steel cylinders (Part 2).
with different surface treatments luted to bovine dentin
Steel cylinders 480 steel cylinders ex. Dentsply
Sirona
2.1.1. Zirconia cylinders and tooth substrates
(6 mm dia. / 2 mm height)
480 cylinders of pre-sintered Prettau® Zirconia (Zirkonzahn
RocatecTM Plus
GmbH, Gais, Italy) were used in this study (see Table 2A). Three
High-purity Al2 O3 110 ␮m, modified
different types of surface pretreatment of zirconia cylinders
Air abrasion of steel with silica (SiO2 )
cylinders Pressure 3.5 bar were applied:
Duration 5−7 s (i) a group using tribochemical silica coating using air abra-
Distance 10 mm sion with “RocatecTM Soft” (see 2.1.2), (ii) a group where the
Angle 45◦ “glaze on technique” with additional air abrasion was applied
Priming of Rocatec Clearfil Ceramic Primer Plus (CCPP) (see 2.1.3.), and (iii) a control group with no surface pretreat-
Plus treated steel Applied with an applicator brush for
ment (see 2.1.4.). Groups (i) and (iii) received a coating with
cylinders 20 s
468 d e n t a l m a t e r i a l s 3 7 ( 2 0 2 1 ) 464–476
Fig. 1 – (A) Test variables of part 1 (B) Test variables of part 2.
either a ceramic primer, an universal primer or no coating
before the application of the RCCs.
480 bovine teeth were embedded in round small plas-
tic moulds with Epoxy Resin (EpoFix Resin, Struers GmbH,
Sarasota, Florida, USA). Specimens were stored dry under
a laboratory exhaust hood until they were fully hardened.
Thereafter the embedded teeth were ground on the buccal
side with a grinder/polisher (Metaserv 2000 Grinder/Polisher,
Buehler, Lake Bluff, Illinois) until an adequate dentin surface
was exposed. Papers of different granulation size (P80, P600
and P1200, CarbiMetTM , Buehler, Lake Bluff, Illinois, USA) were
used.
2.1.2. Surface treatment of zirconia cylinders using
tribochemical silica coating
Zirconia cylinders were air-abraded with RocatecTM Soft (R-
TEC) (Rocatec, 3M ESPE, Seefeld, Germany) (see Table 2A).
2.1.2.1. Primers. A ceramic primer (Clearfil Ceramic Primer
[CCP], Kuraray Noritake Dental Inc., Tokio, Japan) or a univer-
sal primer (Monobond-Plus [MBP], Ivoclar Vivadent, Schaan,
Liechtenstein), was applied onto the zirconia cylinders for 60
s and dried carefully with air, making sure they were not over-
dried.
2.1.2.2. Self-adhesive resin composite cements (RCCs). Zirconia
cylinders were luted with the RCCs Maxcem Elite (MCE) (Kerr
Dental, Orange, USA) or RelyX Unicem 2 Automix (RXU) (3M
ESPE, Seefeld, Germany) to bovine dentin. During the setting
period of the cements a constant pressure of 20 g/mm2 was
applied onto the specimens using a custom-made device. For
MCE this pressure was applied for 4 min, for RXU for 6 min,
according to manufacturer’s instructions. First, cements were
irradiated just for 1 s with a light-curing unit (Elipar Deep
Cure-S, 3M ESPE, St. Paul, USA) to remove excess cement.
Thereafter the cements were cured at the contact surface
from three different directions for a total of 60 s. Irradiance
of the curing unit was verified with a MARC-RCTM device (Blue
Light Analytics, Halifax, NS, Canada). The zirconia cylinders
luted to dentin were stored in an incubator (Heraeus incubator
B6200, Thermo Fisher Scientific Inc., Waltham, Massachusetts,
USA) at 37 ◦ C and kept under 100% relative humidity for
24 h to create test conditions similar to the oral environ-
ment.
 d e n t a l m a t e r i a l s 3 7 ( 2 0 2 1 ) 464–476
2.1.3. Surface treatment of zirconia cylinders using “glaze
on” techniques
2.1.3.1. Air abrasion. Zirconia cylinders were initially air-
abraded (protocol see Table 2A) and afterwards cleaned in an
ultrasonic bath (Sonorex digitec, BANDELIN electronic GmbH
& Co. KG, Berlin, Germany) with distilled water for 10 min and
then dried with air.
2.1.3.2. Glazing. The surfaces of the zirconia cylinders were
sprayed until the surface had a uniform layer of glaze. Hotbond
zirconnect Spray (HB) (Dental Creativ Management GmbH,
Rostock, Germany), Zenostar Magic Glaze Spray (ZM) (Wieland
Dental + Technik GmbH & Co. KG, Pforzheim, Germany) and
IPS e.max Ceram Glaze Spray (IPS) (Ivoclar Vivadent, Schaan,
Liechtenstein) were used for glazing. Zirconia cylinders were
then fired in a dental ceramic furnace (Programat® CS2,
Ivoclar Vivadent, Schaan, Liechtenstein) according to the man-
ufacturer’s specifications. After cooling, the cylinders were
air-abraded again, using a different protocol depending on the
test group (see Table 2A) and cleaned again in an ultrasonic
bath. During the experimental study, ZM was removed from
the market without prior notice. Therefore, the experiments
were continued with a similar product, IPS e.max Ceram Glaze
Spray (IPS).
2.1.3.3. HF-treatment. Surfaces of zirconia cylinders of the
groups HB and ZM were etched with hydrofluoric acid 9%
(Ultradent® Porcelain Etch, Ultradent Products GmbH, Köln,
Germany) for 60 s and rinsed under running water for 30 s and
dried with air. Specimens of IPS were etched for 30 s.
2.1.3.4. Universal primers. After HF-treatment zirconia cylin-
ders received coating with one of the two universal primers
used in this study (see 2.1.2.1.)
2.1.3.5. Self-adhesive resin composite cements. Thereafter zir-
conia cylinders were bonded with one of the two RCCs used in
this study (see 2.1.2.2).
2.1.4. Controls
2.1.4.1. Surface treatment. None of the three surface treat-
ments applied elsewhere in this study (tribochemical coating,
air abrasion, glaze on technique with HF-treatment) were
applied to the controls.
2.1.4.2. Universal primers. For the control groups, zirconia
cylinders were treated either with the primers used in this
experiment (see 2.1.2.1.) or received no primer treatment.
2.1.4.3. Self adhesive resin composite cements. See 2.1.2.2
2.2. Part 2: Influence of different surface treatments of
zirconia cuboid substrates on the adhesion of
self-adhesive cements
2.2.1. Steel cylinders bonded to zirconia cuboid substrates
480 zirconia cuboid substrates (Y-TZP CERCON ht, Dentsply
Sirona, Bensheim, Germany) were used in this study (Table
2A). Again, three different types of surface pretreatments of
the zirconia substrates were applied:
469
(i) four different air abrasion protocols (see 2.2.2), (ii) one
“glaze on” technique (see 2.2.3) and (iii) a control group with
no surface pretreatment (see 2.2.4.). Groups (i) and (iii) received
a coating with two different universal primers or no coat-
ing before the application of the self-adhesive composite
cements.
Steel cylinders (ø 6 mm, cylinder height 2 mm, Dentsply
Sirona, Bensheim, Germany) were pretreated with RocatecTM
Plus (3M ESPE, Seefeld, Germany) followed by treatment with
Clearfil Ceramic Primer Plus (CCPP) (Kuraray Noritake Dental
Inc., Tokyo, Japan), which also serves as a metal primer, for
20 s. Cylinders were then cleaned with oil-free air followed by
treatment in an ultrasonic bath for 10 min. Afterwards steel
cylinders were fixed on the zirconia cuboids, following Wiedig
et al. [15] (Table 2B), using two different composite cements as
described below.
2.2.2. Surface treatment of zirconia cuboids with air
abrasion
Zirconia cuboids were air-abraded using 4 different protocols
(see Table 2A), cleaned in an ultrasonic bath with distilled
water for 10 min and then dried again with oil-free air.
2.2.2.1. Electron microscope examination. Randomly selected
zirconia cylinders were examined using an environmental
scanning electron microscope (FEI ESEM Quanta 200, FEI Com-
pany, Hillsboro, Oregon, USA) before and after air abrasion
(Fig. 2A–E).
2.2.2.2. Universal primers. Half of the air-abraded zirconia
cuboids were treated with the respective primer of the
adhesive system, Prime&Bond active (PBA) (Dentsply Sirona,
Bensheim, Germany) or CCPP for 20 s followed by air drying.
2.2.2.3. Self-adhesive resin composite cements. After surface
conditioning, the steel cylinders were bonded onto the zir-
conia cuboids using either Calibra Universal (CAU) (Dentsply
Sirona, Bensheim, Germany) or PANAVIA SA Cement Plus
(PSA) (Kuraray Noritake Dental Inc., Tokyo, Japan). For bond-
ing procedure, again a custom-made device was used as
described above (2.1.2.2.). Cements were photo-activated
using an EliparTM S10 curing light (3M ESPE, St. Paul, USA)
as described above (2.1.2.2.). Again, irradiance of the curing
unit was verified with a MARC-RCTM device. To ensure curing
even on the non-exposed surfaces, the luted test specimens
(including the weighting device) were placed in an incubator
at 37 ◦ C for 6 min, and afterwards stored in distilled water at
37 ◦ C in the incubator for 7 days before shear bond strength
measurements according to Bielen et al. [16].
2.2.3. Surface treatment of zirconia cuboids with glaze-on
technique
Zirconia cuboids were air-abraded using only one protocol
(see Table 2A), and afterwards cleaned as described above (see
2.2.2.).
2.2.3.1. Glazing. In part 2 all zirconia cuboids were sprayed
only with HB. Application and firing protocols were applied
according to the manufacturer’s instructions (see Table 2A). In
470 d e n t a l m a t e r i a l s 3 7 ( 2 0 2 1 ) 464–476

Fig. 2 – (A–E) SEM images of zirconia surfaces after air abrasion with Al2 O3 using four different protocols and without air
abrasion (control).
(A) Group 1: Particle size 110 ␮m; Pressure 3.5 bar.
(B) Group 2: Particle size 110 ␮m; Pressure 2 bar.
(C) Group 3: Particle size 50 ␮m; Pressure 2 bar.
(D) Group 4: Particle size 50 ␮m; Pressure 0.5 bar.
(E) Control group without air abrasion.

the next step, the glass-ceramic coating was again air-abraded
and cuboids were cleaned again in an ultrasonic bath.
2.2.3.2. HF-treatment. All zirconia cuboids glaced with HB
were subsequently air-abraded and etched with HF.
2.2.3.3. Silanization/Priming. Silanization of HF-treated zirco-
nia cuboids was carried out using Calibra Silane (CAS) for 30
s or CCPP for 20 s. A moist wetting of the entire surface was
ensured continuously by means of a microbrush, if necessary,
the amount of adhesion promoter was increased during the
 d e n t a l m a t e r i a l s 3 7 ( 2 0 2 1 ) 464–476 471

exposure time. Subsequently, the solvent residues were dried 2.2.4. Controls
with a multifunctional syringe. 2.2.4.1. Surface treatment. None of the surface treatments
applied in this study (air abrasion or glace-on technique) were
2.2.3.4. Bonding. In the next step an adhesive, Prime&Bond conducted for the controls.
active (PBA) or Clearfil universal bond quick (CUBQ) was
applied to half of the zirconia cuboids. Continuous wetting
was maintained for 20 s using a microbrush. Excess solvent
2.2.4.2. Universal primers. In the control group, zirconia
was blown off with a multifunctional syringe
cuboids were either treated with the primers used in this
experiment (see 2.2.2.2.) or received no primer treatment.
2.2.3.5. Self-adhesive resin composite cements. After surface
conditioning, the metal cylinders were bonded to the zirconia
cuboids either with CAU or PSA and stored before measure-
ments as described in 2.2.2.3. 2.2.4.3. Self adhesive resin composite cements. See 2.2.2.3.

Fig. 3 – (A) Schematic of shear device for part 1. (B) Schematic of shear device for part 2.
472 d e n t a l m a t e r i a l s 3 7 ( 2 0 2 1 ) 464–476

2.3. Shear bond strength measurements

The shear bond strength measurements for both parts were

operated with a Zwick universal testing machine (Type 1486,
Zwick Roell, Ulm, Germany). The luted specimens were fixed
in a shear testing device (Fig. 3A and B) [17] and afterwards
loaded with a crosshead speed of 0.8 mm/min until failure.
The breaking load was measured and stated in stress units
(MPa).

2.4. Statistical methods

Two-way ANOVAs were applied evaluating shear bond

strength (SBS) by the factors pretreatment, primer, bonding,
or cement respectively, as well as their interaction. Residual
diagnostics showed reasonable approximation of normality,
but considering the relatively high sample size (total 480 for
each part of the study, at least 20 in any sub-group) even relying
on the central limit theorem should be sensible.
Post-hoc tests were done using Tukey’s Honest Significant
Difference (HSD) method, thereby controlling for multiple test-
ing.
All computations were done using R version 4.0.2 (R Core
Team 2020)

3. Results

3.1. Part 1: Shear bond strength of zirconia cylinders

with different surface treatments luted to bovine dentin

Shear bond strengths of the interface when zirconia surfaces

were treated with RocatecTM Soft were significantly higher
than the controls (specimens without pretreatment) (p < 0.001,
Fig. 4A). Values from all “glaze on” techniques were not signif-
icantly different from each other and from controls (Fig. 4A).
Pretreatment of zirconia surfaces with both primers showed
significantly higher SBS than the controls (p < 0.01, control vs
CCP p < 0.001; control vs MBS p = 0.007 (Fig. 4B). Cementations
with RXU showed significantly higher SBS than with MCE (p <
0.001, Fig. 4C).

(C) Shear bond strengths (MPa) of zirconia cylinders, luted

to bovine dentin after air abrasion with RocatecTM Soft or
without air abrasion, treated with the respective primer
(Clearfil Ceramic Primer or Monobond-S) or without primer.
Comparison of the two applied self-adhesive composite
cements Maxcem Elite (MCE) or RelyX Unicem 2 Automix
Fig. 4 – (A) Shear bond strengths (MPa) of zirconia cylinders (RXU).
with different surface treatments luted to bovine dentin. (B) R-TEC = RocatecTM Soft
Shear bond strengths (MPa) of zirconia cylinders, luted to Control = No surface treatment
bovine dentin after air abrasion with RocatecTM Soft or IPS = IPS e.max Ceram Glaze Spray
without air abrasion, treated with the respective primer ZM = Zenostar Magic Glaze Spray
(Clearfil Ceramic Primer or Monobond-S) or without primer. HB = Hotbond zirconnect Spray
CCP = Clearfil Ceramic Primer
MBS = Monobond-S
 d e n t a l m a t e r i a l s 3 7 ( 2 0 2 1 ) 464–476
Fig. 5 – (A) Shear bond strengths (MPa) of zirconia cuboids
luted to steel cylinders. Cuboids were treated with Hotbond
zirconnect Spray (HB) or air-abraded using four different
protocols concerning applied pressure and particle size of
Al2 O3 . (B) Shear bond strengths (MPa) of zirconia cuboids
luted to steel cylinders after air abrasion, using four
473
3.2. Part 2: Influence of different surface treatments of
zirconia cuboid substrates on the adhesion of
self-adhesive cements
Shear bond strength between RCC-bonded steel cylinders and
zirconia surfaces glazed with HB was not significantly dif-
ferent from controls (Fig. 5A). All investigated air abrasion
protocols increased the SBS (p < 0.0001), but there was no sig-
nificant difference between the protocols (Fig. 5A). Examples
for the different air abrasion protocols are shown in Fig. 2A–E.
Again, pretreatment of zirconia surfaces with both primers
showed significantly higher SBS than the controls (p < 0.001,
Fig. 5B). A significant difference between the cements with dif-
ferent formulations was observed. When zirconia specimens
were air abraded regardless of which protocol was applied,
highest SBS were obtained with CAU with PBA. CAU without
PBA exhibited the lowest SBS (Fig. 5C). When zirconia spec-
imens were glazed with HB, PSA with CCPP with or without
bonding (CUBQ) showed higer SBS than CAU with CAS with or
without bonding (PBA) (Fig. 5D). When specimens were treated
with HB and hydrofluoric acid and silane (CCPP or CAS) after-
wards, additonal coating with a bonding (CUBQ or PBA) did not
influence the SBS.
3.2.1. Failure mode
In 98% of all tested specimens failures occurred between zirco-
nia and cement, in 0.8% between cement and metal cylinders
and in 1.2% mixed failures were detected.
4. Discussion
It has been shown that results achieved by bond strength
tests (e.g. tensile or shear bond methods) depend not only
on the materials involved but also on the geometry of the
test arrangement [18]. Usually important details of the test
arrangement are not reported so that accurate analysis of the
applied method, reproduceability and comparison with other
studies in the literature are not possible [18–20]. Following
different protocols, or without air abrasion, treated with the
respective primer (Prime&Bond active or Clearfil Ceramic
Primer Plus) or without primer. (C) Shear bond strengths
(MPa) of zirconia cuboids luted to steel cylinders after air
abrasion, using four different protocols, or without air
abrasion. Comparison of the two applied self-adhesive
cements in combination with their respective primers or
without primer. (D) Shear bond strengths (MPa) of zirconia
cuboids luted to steel cylinders. All zirconia cuboids were
initially treated with Hotbond zirconnect Spray (HB).
Comparison of the two applied self-adhesive cements in
combination with their respective primers with bonding
applied after priming or without bonding.
CAU = Calibra Universal
PSA = PANAVIA SA Cement Plus
CCPP = Clearfil Ceramic Primer Plus
PBA = Prime&Bond active
CAS = Calibra Silane
CUBQ = Clearfil universal bond quick
474 d e n t a l m a t e r i a l s 3 7 ( 2 0 2 1 ) 464–476
these recommendations, we have presented all variables of
this study in Tables 2A and 2B. In part 1 of this study we
used bovine teeth, which have been shown, by meta-analysis,
to function as a reliable substitute for human teeth for bond
strength studies [21].
In part 1 of this study, specimens were stored at 37 ◦ C
under 100% relative humidity for 24 h before testing, but
the failures were mixed, i.e. failures occurred partly between
cement/dentin and between cement/zirconia in the same
test specimens. Therefore, in part 2, a different experimen-
tal protocol was chosen, using stainless steel discs bonded
to zirconia with RCCs, expecting that adhesive failures would
occur mainly between RCC/zirconia, rather than at the SS/RCC
interface, which was the case in 98% of all shear tests. Adhe-
sive bond strength is most commonly evaluated by Macro
SBS or TBS tests [22,23], with the option to rank the mate-
rials [3], although their interpretation is often questioned
[18,22,23].
In part 2, for the minimal storage time of specimens before
testing, a different protocol of 7 days was considered beneficial
and more clinically relevant [10,16]. This allowed for complete
curing of the resin cements. The increase in hardness after
irradiation (a measure of curing) is rapid in the first hour;
thereafter it slows down reaching a maximum value within 24
h [24]. However, it has been shown that long-term water stor-
age or even thermocycling (e.g 10000 cycles) only had a small
effect on bonding to zirconia [10,25]. Rough surfaces with dif-
ferent profiles may contribute differently to the magnitudes of
shear bond strengths as these evalute more the micromechan-
ical retention at the interface than any chemically promoted
adhesion. Practically speaking, however, it is the increased dis-
ruption force that matters, rather than the specific interfacial
bonding mechanism.
The results of parts 1 and 2 gave complementary insights.
In both parts “Glaze on” techniques did not improve SBS (null
hypothesis (i) was accepted), while all applied air abrasion pro-
tocols resulted in higher SBS (null hypothesis (ii) was rejected).
Pretreatments of surfaces with zirconia primers also led to
higher SBS (null hypothesis (iii) was rejected). The different
brands of the cements also had a significant impact on the
SBS (null hypothesis (iv) was accepted).
Due to the aesthetic demands of patients, zirconia restora-
tions are increasingly replacing precious metal restorations
[26]. Compared to precious metal restorations, the friction of
zirconia workpieces is usually lower. Therefore, conventional
cementation with zinc phosphate cement is in some cases
insufficient [27–32]. There have been several attempts to create
a strong and durable bond between oxide ceramic restorations
and dentin. Various surface treatments of zirconia have been
developed for more than 20 years [4].
Zirconia cannot be etched or treated with silanization alone
due to its lack of silica phases [10,33]. Decisive for success-
ful long-term bonding of composite luting cements to oxide
ceramic restorations is the micromechanical and chemical
retention and interaction between these two surfaces [3,7,10].
One approach is surface coating to establish a silica layer,
either by grit blasting, plasma spraying, glass fusing (Inter-
nal coating and “Glaze-On”), or Selective Infiltrative Etching
and nanostructured alumina coating [1,7]. Several studies with
glaze-on techniques showed promising results [6,9,33–35],
using either overglazes, glazes, glass-bead gel, medium fusing
porcelain or a paste liner.
In this study (both in parts 1 and 2), no difference was found
between the different glaze-on techniques and the control,
in line with Thammajaruk et al. [36]. In contrast, Valentino
et al. [37] and Vanderlei et al. [38] determined significantly
increased adhesion with a glass-ceramic glaze in comparison
to conventional grit blasting protocols.
The considerable additional effort involved in the applica-
tion of the “glaze on” techniques, compared to air abrasion,
with no significant effect indicates a low practical benefit.
Air abraded specimens were tested with or without zirconia
primers. In part 2, Panavia SA applied without its respective
primer (CCPP) shows siginificatly higher SBS than Calibra uni-
versal without primer (PBA). This might be caused by the fact
that Panavia SA contains MDP, whereas Calibra does not. On
the other hand, Calibra applied with PBA showed significantly
higher SBS than Panavia SA with CCPP.
Three out of four primers, which have been used for
this present study: Clearfil Ceramic Primer, Clearfil Ceramic
Primer Plus and Monobond Plus, contain MDP and also a spe-
cial bi-functional molecule for silanization. Applying primers
containing silanes can modify the bond strength, since two
studies, which used a technique similar to the “glaze-on” tech-
nique, also investigated the failure mode and concluded that
a silane coupling agent could successfully establish a bond
between the silica containing layer and the used resin lut-
ing cements by creating a durable siloxane network [6,33].
According to Martins et al., the silane molecules are able to
bond to the hydroxyl groups (OH) of the silica-based surface
and are co-polymerized within the matrix of resin composite
cements [33]. In this study, according to the results of But-
ler et al. [39], the use of a primer increased SBS compared to
groups that were bonded without a primer. Without consid-
ering RCCs and surface treatments of the materials, surfaces
treated with primers had significantly higher SBS than sur-
faces bonded without primers.
By air abrading the zirconia specimens with aluminium
oxide corundum, in different grain sizes and with different
air pressures, significantly higher SBS could be achieved com-
pared to the untreated control groups, in line with Byeon
et al. [40]. This is due to a supposed surface enlargement by
the corundum particles, which abrade part of the homoge-
neous smooth surface of the zirconia, depending on the grit
blasting protocol. As a desirable side effect, the surface was
also cleaned and possible contaminations were eliminated, as
described in Yang et al. [41].
A controversial point of surface treatment with grit blasting
is the transformation of the phase. The microdefects men-
tioned above cause compressive stress zones on the surface
of the zirconia, which were observed by Özcan et al. [11] to
increase the flexural strength of the ceramic. However, such a
phase transformation from tetragonal to monoclinic can only
occur once and is an irreversible effect that serves as a kind
of buffer against sudden overload [13]. Aurelio et al. [42] found
that an increase in flexural strength is a positive effect, which,
however, has not yet been sufficiently researched in clini-
cal cases. Furthermore, it is described that flexural strength
increased independent of grain size, air pressure, duration and
aging compared to an untreated control group [42].
 d e n t a l m a t e r i a l s 3 7 ( 2 0 2 1 ) 464–476
In addition to SBS obtained by Byeon et al. [40], it was
found in this study that there were no significant differences
between the various grit blasting protocols applied. Özcan
et al. [12] recommended not to use grain sizes larger than 50
␮m and to apply air pressure with a maximum of 2.5 bar due
to the danger of phase change. For Aurelio et al. [42], however,
this risk was not considered critical.
Overall, this means that pre-treatment with grit blasting
(air abrasion) protocols achieves significantly higher SBS. Due
to the risk of phase transformation described in Özcan et al.
[11], the grit blasting protocol with 50 ␮m particle size and an
air pressure of 0.5 bar is probably the best choice, also consid-
ering that in this study all applied grit blasting protocols gave
good and comparable results.
5. Conclusion
Both complex systems studied: zirconia / RCC / bovine dentin
(part 1) and the RCC / zironia interface (part 2) led to consistent
results.
All applied air abrasion protocols improved the bond
strengths, whereas “Glaze-on” surface treatments did not
demonstrate any significant improvement. Air abrasion with
Al2 O3, 0.5 bar and 50 ␮m particle size might be the best choice
with minimal risk for phase transformation. Coating zirconia
with primers (with or without MDP) led to a further increase
of shear bond strengths.
Acknowledgements
We would like to thank Sonia Arellano, Nikolaus Maderbacher
and Hassan Ali Shokoohi Tabrizi for skilful technical support
and Dentsply Sirona Deutschland GmbH for supporting this
study in part and Zirkonzahn GmbH for supporting this study
with materials in part.
Appendix A. Supplementary data
Supplementary material related to this article can be
found, in the online version, at doi:https://doi.org/10.1016/
j.dental.2020.12.001.
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