RESEARCH AND EDUCATION

Effect of a zirconia primer on the push-out bond strength of

zirconia posts to root canal dentin
Mahshid Torabi Ardakani, DDS,a Rashin Giti, DDS,b Masume Taghva, DDS,c and Samane Javanmardi, DDSd

Excessive loss of coronal tooth ABSTRACT

structure and insufficient re- Statement of problem. The retention of zirconia ceramic posts to root canal dentin with resin-
maining root structure for the based luting cements is relatively poor.
retention of restorative mate-
Purpose. The purpose of this in vitro study was to evaluate the effect of a new zirconia primer, a
rials necessitate the use of a
mixture of organophosphate and carboxylic acid monomers, on the push-out bond strength of
post and core in some end- zirconia posts to root canal dentin.
odontically treated teeth.1
Selecting the optimum restora- Material and methods. The root canals of 40 extracted human maxillary central incisors were
endodontically treated and the post spaces were prepared. Zirconia posts were luted with 2
tion for endodontically treated
different resin luting agents (Panavia F and Clearfil SA luting cements) with and without the zirconia
anterior teeth is determined by primer (Z-Prime Plus; Bisco). Three segments, each 2 mm high, were cut perpendicular to the post
the demands of esthetics and from each root. Bond strength was determined by pushing out the post with a universal testing
strength.2-4 Cast gold posts have machine. Three-way ANOVA and the Tukey HSD test was used to assess the effects of the zirconia
a long-term clinical success primer, the 2 different resin luting cements, and different thirds of the root canal (a=.05).
rate.5,6 With translucent ceramic Results. The zirconia primer significantly increased the push-out bond strength of zirconia posts to
crowns, the effect of the abut- root canal dentin. Clearfil SA luting cement provided significantly higher bond strength than did
ment shade on the final shade of Panavia F. For all experimental groups combined, bond strength decreased from the coronal to
the restoration is a concern. In a the apical section.
ceramic crown with less than 1.6 Conclusions. A zirconia primer based on organophosphate/carboxylic acid monomers
mm thickness, the color of the increased the bond strength of zirconia posts to root canal dentin bonded with both resin luting
underlying core might affect the cements. (J Prosthet Dent 2015;-:---)
esthetics of the definitive resto-
ration.7 Root discoloration and a blue-gray effect on the post retention is one of the most common reasons for the
gingival tissues are another esthetic consequence of cast failure of post-retained restorations.18,19 Accordingly,
8,9
posts. clinicians need to be aware of the bond strengths of
The wide range of esthetic post systems, including various posts and their retention in order to reduce the
fiber-reinforced composite resin posts and zirconia risk of root fracture. The use of adhesive cements to
ceramic posts, are available.10-12 The use of zirconia as a cement post materials in the root canal can reinforce the
post and core material was first introduced in 199313 tooth structure and improve the retention of the post and
because of its excellent mechanical properties, including the crown.20,21 To improve the bonding of resin cements
high chemical stability, modulus of elasticity, and to silica ceramics, hydrofluoric acid (5-9.5%) is used to
strength, as well as its esthetic properties.14-17 The loss of produce a porous surface, followed by the application of a

Supported by the Vice-Chancellory of Research, Shiraz University of Medical Science (grant 6329). This article is based on the thesis by R.G.
a
Private practice, Shiraz, Iran.
b
Resident, Department of Prosthodontics, School of Dentistry, Shiraz University of Medical Sciences, Shiraz, Iran.
c
Resident, Department of Prosthodontics, School of Dentistry, Shiraz University of Medical Sciences, Shiraz, Iran.
d
Resident, Department of Endodontics, School of Dentistry, Shiraz University of Medical Sciences, Shiraz, Iran.

THE JOURNAL OF PROSTHETIC DENTISTRY 1

2 Volume
Clinical Implications
This in vitro study suggests that the application
of a zirconia primer based on organophosphate/
carboxylic acid (Z-Prime Plus) with resin luting
cements can improve the bond strength of zirconia
posts to root canal dentin.
silane coupling agent to form a siloxane network with the
silica in the ceramic material.22 However, this reaction is
not effective for zirconia ceramics because of the lack of a
silica phase.23-25 Specific monomers have been devel-
oped to improve the zirconia bond to adhesive resins,
including 10-methacryloxy decyl dihydrogen phosphate
(MDP),26-29 4-methacryloxy ethyl trimellitic anhydride
(4-META), and other monomers.30,31 A new approach to
improving the zirconia-resin bond strength involves
mixing organophosphate and carboxylic acid monomers
to form a zirconia primer. The organofunctional part of
organophosphate monomer can be copolymerized with
the monomers of resin luting agents, and its phosphoric
acid groups are thought to create a bond with the metal
oxide in zirconia.32 The other monomer in this primer is a
carboxylic acid, which also contributes to the develop-
ment of the bond.33
Because no study had focused specifically on this issue,
the current study was designed to evaluate the effect of this
zirconia primer (Z-Prime Plus; Bisco Inc) on the push-out
bond strength of zirconia posts to root canal dentin with
2 different adhesive resin cements. The first test null hy-
pothesis was that the Z-Prime Plus primer cannot enhance
the bond strength of zirconia posts to root canal dentin.
The second test null hypothesis was that the bond strength
of zirconia posts to root canal dentin does not vary between
the 2 resin luting cements. The third null hypothesis was
that the bond strength of zirconia posts to root canal dentin
does not vary regionally.
MATERIAL AND METHODS
Forty single-rooted human maxillary permanent central
incisors were used, after receiving approval from the
ethics committee of Shiraz School of Dentistry. These
teeth had been recently extracted from patients who
required periodontal treatment. The inclusion criteria
were absence of root caries or cracks and a 13 mm root
length. Each tooth was decoronated with a double-faced
diamond disk (DeguDent GmbH) 2 mm coronal to the
cement-enamel junction. All root canals were instru-
mented by an endodontist (S.J.). The root canals were
irrigated with 3% NaOCl, cleansed, and shaped with
nickel-titanium rotary instruments (size S1, S2, and F3,
Protaper; Dentsply Maillefer). Then the root canals were
THE JOURNAL OF PROSTHETIC DENTISTRY
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rinsed with distilled water, dried with paper points, and
obturated with gutta percha (Guttapercha; Ariadent) by
using AH Plus sealer (AH Plus; Dentsply Maillefer).
After endodontic treatment, the teeth were stored in
water at room temperature (23 ±1 C) for 24 hours. Post
spaces were prepared with the specific drills for the 1.4 mm
zirconia posts (Cosmopost; Ivoclar Vivadent AG) produced
by the manufacturer. A minimum of 4 mm of root filling
material remained in the apical part of the root canals.
After post space preparation, the root canals were rinsed
with 5 mL of distilled water to remove the debris and dried
with paper points (Paper Points; Ariadent). Specimens
were divided into 4 groups (n=10) according to the type of
adhesive cement and whether zirconia primer was applied
on the zirconia posts as follows, ZP, zirconia primer+-
Panavia F; ZC, zirconia primer+Clearfil SA luting cement;
P, Panavia F; and C, Clearfil SA luting cement. Table 1
summarizes the materials used in this study.
The root canal dentin was etched for 15 seconds with
37% phosphoric acid gel (Denfil Etchant; Vericom Co
Ltd) and rinsed for 1 minute with water. Excess water
was removed with paper points without desiccating the
dentin. For the ZP and ZC groups, zirconia posts were
treated with an experimental zirconia primer and left
undisturbed for specific times (reaction time) according to
the manufacture’s instruction.
The Panavia F resin luting system was used to bond
zirconia posts to root canal dentin in the ZP and P
groups. For these groups, equal amounts of ED primer
liquids A and B were mixed and applied inside the canal
with a brush and allowed to stand for 60 seconds. Equal
amounts of Panavia F paste A and B were then mixed
and applied to the canal with a Lentulo spiral drill (Mani
Inc, Japan). The zirconia posts were covered with resin
cement and seated to full depth with finger pressure.
Excess cement was removed, and the teeth were poly-
merized for 40 seconds with a light-polymerization unit
(Radiplus LED; SDI) at 1200 mW/cm2 on the cervical
surface of the root canal in the direction of the long axis
and obliquely on the buccal and lingual surfaces.
For the specimens in the ZC and C groups, zirconia
posts were cemented with the self-adhesive Clearfil SA
luting cement. This cement was mixed according to the
manufacturer’s instructions and applied to the root ca-
nals with a spiral paste filler (Lentulo; Z-Prime Plus;
Bisco). The seated posts were polymerized with the
technique used for Panavia F after post insertion.
After 24 hours, each root was sectioned perpendicu-
larly to its long axis with a precision saw (Isomet; Buehler
Ltd) at low speed under cooling water to make 4 root
segments 2 mm in thickness. The first slice was not used
because it contained coronal dentin. The remaining
segments represented the coronal, middle, and apical
thirds of the roots (Fig. 1).
Torabi Ardakani et al
- 2015 3

Table 1. Materials used and their characteristics

Name Type of Material Main Composition Manufacturer Batch No.
Cosmopost Zirconia post Zirconia ceramic Ivoclar Vivadent AG S12653
Z-Prime Plus Zirconia-alumina-metal primer Organophosphate monomer, carboxylic Bisco Inc 1200001555
acid monomer, other monomers
Panavia F Adhesive resin cement HEMA, MDP, 78w% silanized silica and Kuraray Medical Inc 051124
silanized colloidal silica
Clearfil SA luting cement Self-adhesive resin cement Bis-GMA, MDP, TEG-DMA silanized barium glass, Kuraray Noritake Dental Inc 0359AC
silanized colloidal silica

Figure 1. Sectioning of post specimens for push-out test.

The thickness of each root segment was checked with a

digital caliper (Mini Electronic Caliper; Insize Co Ltd). The
specimens were submitted to a micro-push-out test on a
universal testing machine (Z020; Zwick/Roell). A
compressive load was applied at 1 mm/min in the apico-
coronal direction until failure occurred (Fig. 2). The bond
strength was calculated in MPa by dividing the load at
failure (N) by the area (mm2) of the bonded interface. The
surface area of the bonded surface was calculated using the
equation A=2pr×h, where A is the area of the bonded
interface, p=3.14, r is the radius of the post segment (mm),
and h is the thickness of the root segment (mm).34
Three-way ANOVA was used to assess the effects of
the zirconia primer, different resin luting cements, and
different sections of the root canal in this context. The
Tukey HSD test was used for pairwise comparisons of
Figure 2. Sectioned specimen positioned in mechanical testing machine
different root segments. Software (SPSS 15.0; IBM Corp)
for push-out test.
was used for statistical analysis (a=.05).

RESULTS The mean push-out bond strength in the coronal

section (17.2 ±6.94 MPa) was significantly greater than in
The mean push-out bond strength values (MPa) and
the middle (11.09 ±6.46 MPa) (P<.001) and apical (7.43
standard deviations for each group are listed in Table 2.
±5.53 MPa) (P<.001) sections. The push-out bond
All specimens fractured predominantly at the interface
strength in the middle section was significantly higher
between the post and resin luting cement. The mean
than in the apical section (P=.025).
push-out bond strength for groups using the zirconia
primer was 14.57 ±7.25 MPa, significantly higher than
DISCUSSION
the mean value in the other groups (9.28 ±6.78 MPa)
(P<.001). Clearfil SA luting cement had significantly This study evaluated the effect of an organophosphate/
greater push-out bond strength (13.44 ±5.26 MPa) than carboxylic acid primer on the push-out bond strength of
Panavia F (10.41 ±8.9 MPa) (P=.008). zirconia posts to root canal dentin with 2 different resin

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Table 2. Mean ±SD of push-out bond strength (MPa) in experimental groups
Clearfil SA Luting Cement
Section With Zrp (ZC)
Coronal 18.8 ±6.3aA
bA
Middle 13.8 ±3.2
Apical 13.4 ±4.3cA
Zrp, Zirconia primer; ZP, Panavia F+Zrp; ZC, Clearfil SA luting cement+Zrp; P, Panavia F; C, Clearfil SA luting cement.
Groups identified by different lowercase letters in each column are significantly different (P<.05); groups identified by different uppercase letters in each row are significantly different (P<.05).
luting cements. The results supported the first hypothesis
that the zirconia primer enhanced the push-out bond
strength of zirconia posts to root canal dentin.
Various studies have used different mechanical and
chemical surface treatments to improve the bond strength
of zirconia ceramics to resin cements.12,15,22,35 Sahafi et al9
reported that Cojet treatment (silicate-coated particles of
30 mm, silane) most increased the bond strength of zirconia
posts to root canal dentin. However, etching with hydro-
fluoric acid (with or without silane treatment) decreased the
bond strength of zirconia posts to root dentin.9 Some
studies reported that airborne-particle abrasion with
aluminum oxide (Al2O3) significantly increased the bond
strength of zirconia to resin cement by roughening the
surface. The treatment also induced a tetragonal to mono-
clinic phase transformation and consequently increased the
strength of zirconia.15,22,35 However, de Oyagüe et al16 did
not find a higher bond strength after airborne-particle
abrasion; the zirconia surface became rougher than the
control group without increasing bond strength. One of the
most common chemical surface treatments tested was
hydrofluoric acid; most studies showed that etching with
hydrofluoric acid did not increase the bond between zirco-
nia and adhesive resins because of the absence of the glassy
matrix in zirconia.24,25,35
Different types of monomers and primers are known to
increase the bond strength of zirconia ceramics,26-29 and
some adhesive monomers like MDP and 4-META (present
in some luting agents and metal primers) were found to
have better adhesion to ZrO2 because these acidic mono-
mers react with the oxide groups on the zirconia ceramic
surface.29 Dias de Souza et al28 reported that different types
of metal primers improved the bond strength between zir-
conia and a self-adhesive resin cement (Rely X Unicem; 3M
ESPE). Few studies have evaluated the effect of the zirconia
primer (a mixture of organophosphate and carboxylic acid
monomer) on the bond strength of zirconia to resin ce-
ments. According to the study by Magne et al,33 a zirconia
primer (Z-Prime Plus) could significantly increase the bond
strength of different resin luting agents (Biscem, Duo-link,
Panavia F). It also could significantly increase the bond
strength of square-shaped yttrium-stabilized tetragonal
zirconium polycrystal (Y-TZP) specimens to resin cement
(Rely X U100; 3M ESPE).31 These studies agree with the
findings of the current study, which showed that this
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Type of Adhesive Cement
Panavia F
Without Zrp (C) With Zrp (ZP) Without Zrp (P)
15.59 ±3.09aA 20.6 ±3.6aA 13.9 ±11.02aA
bB bA
8.6 ±3.5 16.8 ±8.09 4.99 ±0.98bB
10.2 ±4.3bA 3.7 ±1.5cB 2.3 ±0.6cB
zirconia primer significantly increased the bond strength of
zirconia posts to root canal dentin with different resin luting
cements.
The current study also showed that Clearfil SA luting
cement, which is an MDP-containing self-adhesive, had
significantly greater bond strength than Panavia F, which is
a more hydrophobic resin luting cement.36 Yaman et al3 also
showed that the bond strength of Panavia F was lower than
that of the self-adhesive cement (Rely X Unicem) to fiber
and zirconia posts in the root canal. However, Dias de Souza
et al28 found that Panavia F provided a higher bond strength
when bonded to zirconia than did Rely X Unicem. The
bonding of self-adhesive cement seems to depend on both
micromechanical and chemical adhesion to hydroxyapatite.
This chemical reaction could be the reason for a greater
tolerance to the moisture present in the root canal.37 Many
self-adhesive cements have a high tolerance to moisture
because water is formed during the neutralization reaction
of phosphoric acid, methacrylate basic fillers, and hy-
droxyapatite.21 The bond to Panavia F may also be influ-
enced by the priming agent used with the resin luting agent.
The self-etch ED primer used with Panavia F is a 1-step
adhesive that contains significant amounts of water that is
difficult to evaporate from the adhesive. Such water can
create a water-polymerized permeable membrane and
contribute to the degradation of the resin bond.38
The third hypothesis that the bond strengths of zir-
conia posts to root canal dentin do not vary regionally
was rejected. Higher bond strength values were detected
in the cervical third of the root, followed by the middle
and apical thirds. These findings are consistent with
other studies3,19,32 on the bond strength of post systems
in different sections of the root canal. This difference can
be explained by the reduction in the number and distri-
bution of dentinal tubules from the cervical to apical re-
gion and the physical difficulties of applying etchants,
primers, and resin cement deep into the apical third.19,32
It may also be related to less effective light polymeriza-
tion and the restriction of resin flow at the apical part of
the root canal.4,39
The results of the present study are not in agreement
with those of Kremeier et al,6 who reported that the bond
strength of endodontic posts increased from the coronal
to the apical sections. They stated that their results were
in contrast to the majority of published reports. When the
Torabi Ardakani et al
- 2015
experimental groups were considered individually, only
for 2 groups (Luscent Anchor/EnaCem and Perma-dor/
Ketac Cem) was the overall increase in bond strength
from the coronal to the apical section statistically signif-
icant; for other groups, the intermediate section had
either a higher or lower bond strength than the
remaining thirds.6
The effects of artificial aging methods such as ther-
mocycling and water storage on the degradation of the
resin-ceramic bond were not evaluated in the current
study and is a limitation of this study.
CONCLUSIONS
Within the limitations of this in vitro study, the organ-
ophosphate/carboxylic acid primer (Z-Prime Plus)
increased the bond strength of zirconia post to root canal
dentin (P<.001). The bond strength of zirconia posts to
root canal dentin was higher with Clearfil SA luting
cement than with Panavia F resin cement (P<.05). The
bond strength of zirconia posts was higher in the coronal
third than in the deeper thirds.
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Corresponding author:
Dr Rashin Giti
Shiraz University of Medical Sciences
Rajayee Boulevard, 21 St
7185933343 Shiraz
IRAN
Email: giti_ra@sums.ac.ir
Acknowledgments
The authors thank Dr Vosough of the Dental Research Development Center, of
the School of Dentistry for the statistical analysis.
Copyright © 2015 by the Editorial Council for The Journal of Prosthetic Dentistry.
THE JOURNAL OF PROSTHETIC DENTISTRY