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Comparison of 2 self-adhesive resin cements with or without a self-etching

primer

Article in General Dentistry · January 2020

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Comparison of 2 self-adhesive resin

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cements with or without a self-etching

primer
Michael R. Meharry, MS, DDS ¢ Jaclyn Schwartz, MS, DMD ¢ Andrew Montalvo, DMD ¢ Dustin Mueller, BS
John C. Mitchell, PhD

Self-adhesive resin cements that eliminate the primer

step have been introduced to simplify the bonding
protocol for indirect restorations. The aim of the present
study was to compare the shear bond strengths (SBSs)
of 2 self-adhesive resin cements used with or without
W hen seeking satisfactory bond strengths to pro-
vide longevity to indirect restorations that are
costly for patients, dentists must be careful not
to sacrifice bond integrity for the sake of simplification and
speed. Manufacturers of self-adhesive resin cements claim
a self-etching primer. The hypothesis was that add- that their cement formulas eliminate the need to pretreat the
ing a separate primer component to the self-adhesive tooth, reducing the potential for errors in etching, priming,
systems would increase the SBS at the tooth-adhesive and bonding.1,2 Manufacturers also promote studies show-
interface. One hundred twenty extracted human molars ing that the bond strengths of their products to dentin and
were hemisectioned and embedded in epoxy. Specimens enamel are comparable to those of systems that use prim-
were polished to expose enamel or dentin surfaces and ing and/or bonding components.1,2 Powers described the
randomly assigned to 12 test groups (n = 20). The tested properties and manipulation of self-adhesive resin cements.3
variables were (1) the type of bonded tissue (enamel or However, the use of a separate primer may increase the
dentin); (2) the cement used; (3) whether the cement bond strength and provide higher success rates and better
was applied with or without a primer; (4) and whether longevity for restorations. The results of several studies have
the primer was air dried or photopolymerized. Bonding demonstrated that the use of products with a separate primer
jigs were used to apply the self-adhesive resin cement increases the shear bond strength (SBS) of self-adhesive resin
to the tooth surfaces. A 2-minute self-cure was followed cements bonded to zirconia.4-7
by 20 seconds of light curing. Specimens were stored in Testing has also shown that the bond strengths of self-adhesive
water for 24 hours and then subjected to SBS testing in a resin cements increase after aging when the manufacturer’s pro-
universal testing machine. Fractured specimens were ex- tocol is followed.8 However, few studies have evaluated the effect
amined under a microscope to determine the modes of on the shear bond strengths to enamel and dentin when a sepa-
failure. Mean SBS values were compared using a paired rate primer component is added prior to placement of the self-
Student t test (with post hoc Tukey test) and an analysis adhesive resin cement. When combined with existing information
of variance (α = 0.05). Compared to the control groups, about the interface between the cement and tooth structure,
the air-dried primer groups showed SBSs that were 4-6 examination of the cement bond strengths to enamel and dentin
times greater for the specimens bonded to dentin and at the cement interface will provide valuable information about
2-3 times greater for specimens bonded to enamel. The the strength of a restoration.
photopolymerized primer groups followed the same Primers serve the important function of bridging the gap
trend. The photopolymerized groups showed higher between 2 chemically dissimilar components—the hydrophilic
percentages of cohesive tooth failure than did air-dried tooth surface and the hydrophobic restorative material. Primers
primer groups. Placement of a self-etching primer prior aid in micromechanical retention and ionic bonding. The use of
to a self-adhesive resin cement significantly increased separate primers has been shown to significantly increase bond
the SBS to tooth structure of the “all-in-1” resin cements strengths.9 Thus, it seems logical to conclude that the use of a
that were tested. Photopolymerizing the primer did not priming component would yield greater bond strengths than
significantly increase the bond strength. application of the self-adhesive cement system alone.
The primary goal of the present study was to determine if
Received: August 20, 2018 there might be an advantage to adding a separate primer to
Accepted: October 3, 2018 the tooth surface, rather than following the manufacturer’s
simplified 1-step protocol, when a self-adhesive resin cement
Key words: bond strength, bonding primer, resin is used. The hypothesis was that the addition of a separate
cement, self-adhesive primer component to the tested self-adhesive systems would
increase the SBS at the tooth-adhesive interface. A separate
primer, Clearfil SE Protect (Kuraray America) was used in con-
junction with 2 self-adhesive cements, SpeedCEM (SC; Ivoclar
Exercise No. GD450, p. 29 Vivadent) and RelyX Unicem 2 Automix (RU2; 3M ESPE),
Subject code: Basic Science (010) applied to both human enamel or dentin. The mode of failure
was also investigated.

22 GENERAL DENTISTRY January/February 2020

Materials and methods
Freshly extracted human molars were stored in 0.5% chloramine-
T solution in a darkened bottle refrigerated at 4°C. Teeth were
selected primarily by size to ensure that a large flat area was
available to provide ample surface for enamel bonding. A power
analysis of pilot studies determined the appropriate sample size
for statistical significance.

Tooth preparation
One hundred twenty teeth were sectioned using a diamond
disc in a laboratory handpiece. The teeth were cut in half in the
mesiodistal direction. Every few seconds, the teeth were dipped
in cool water to minimize heating. Once the tooth was bisected
to the cementoenamel junction, the disc was used to score
the tooth apical to the cementoenamel junction, allowing the
bisected portion of the crown to be fractured off the root; this
process created 1 bonding surface for enamel and 1 for dentin Fig 1. Specimen bonded to dentin for shear bond strength testing.
from each tooth. Once the teeth were sectioned, 240 bonding
specimens were created. The teeth were embedded in EpoxiCure
2 (Buehler) acrylic using a mold (Ultradent Products).
The epoxy-mounted specimens were polished through 400- light before it was photopolymerized with an LED light-curing
and 600-grit polishing papers, on an EcoMet 250 Pro Grinder unit for 20 seconds. After curing was performed, the specimen
Polisher (Buehler) using copious quantities of water to cool was immediately removed from the bonding jig. This process
and wash away debris and expose a smooth surface of either was repeated until there were 20 specimens in each group.
enamel or dentin. They were stored in deionized water until The specimens were labeled and stored in deionized water for
bonded. Specimens were sorted into groups of exposed enamel 24 hours before testing. Figure 1 depicts a bonded dentin speci-
or exposed dentin and randomly assigned to a group that would men ready for testing.
receive primer or not receive primer. These groups were again
divided and grouped to receive either RU2 or SC self-adhesive Shear testing
resin cement. Cements were purchased from commercially avail- The specimens were tested with a universal testing machine
able stock. (E3000, Instron) at a crosshead speed of 0.5 mm/min. A jig
(Ultradent Products) was used to hold the specimen in align-
Bonding procedures ment for proper application of shear stress. The specimen-
All specimens were rinsed with an air-water syringe for 5 sec- testing order was randomized, and load to failure was recorded
onds and air dried for 5 seconds. Specimens were prepared in for each specimen.
groups of 3—each with the same cement, but 1 without primer
and 2 with primer. All specimens were air dried, and one of the Microscopic analysis
primer specimens was photopolymerized prior to bonding. This The failure mode of the specimens was evaluated using a
process was repeated until all 12 groups for both dentin and microscope (Wild Heerbrugg) with an eyepiece camera (Dino-
enamel (n = 20) were bonded. Eye, AnMo Electronics). Photographs of each specimen were
In the 4 control groups, SC and RU2 were bonded to enamel collected and stored for analysis. The 4 failure modes were
or dentin surfaces according to the manufacturer’s protocol, classified as cohesive failure within the resin, cohesive failure
which was without the use of a separate primer. In 4 test groups, within the tooth, adhesive failure, and mixed adhesive-resin
the primer (Clearfil SE Protect) was applied to the dentin or failure. To reduce bias, the specimens were evaluated at random
enamel surface prior to the application of SC or RU2. The and the failure mode was determined without looking at the
primer was lightly scrubbed onto the bonding surface of the specimen label. In questionable cases, the bonded button was
specimen for 20 seconds and air dried until no fluid movement evaluated for clarification. Specimens that were found to have
was visible, per the primer manufacturer’s instructions. In the been bonded to mixed tissue (enamel and dentin) or enamel and
final 4 test groups, the primer was applied to the dentin or epoxy were excluded from further analysis.
enamel surface as described previously and polymerized for 10
seconds with an LED light-curing unit (Ultra-Lume 5, Ultradent Statistical analysis
Products) prior to bonding with SC or RU2. Specimens were Mean SBS values were compared with a paired Student t test
placed in shear bond strength test mounting jigs (Ultradent (with post hoc Tukey test) to identify differences between
Products) to ensure that consistent specimen geometry was cre- specimens with primer and those without primer (α = 0.05). An
ated for bond testing. This jig allowed for the creation of cement analysis of variance (ANOVA) (α = 0.05) was used to identify
cylinders that were 2.38 mm in diameter and 1.50 mm high. significant differences between and among groups; the tissue
Cement was applied to the specimen through the jig, and the type, adhesive used, use of primer (or not), and use of photo-
cement was allowed to self-cure for 2 minutes under ambient polymerization (or not) were the variables.

agd.org/generaldentistry 23
Comparison of 2 self-adhesive resin cements with or without a self-etching primer

Chart 1. Mean shear bond strengths of enamel groups. Chart 2. Mean shear bond strengths of dentin groups.

35 35

30 30

25 25
Shear bond strength (MPa)

Shear bond strength (MPa)

20 20

15 15

10 10

5 5

0 0
Photo- Air-dried Photo- Air-dried Speed- RelyX Photo- Air-dried Photo- Air-dried Speed- RelyX
polymerized primer polymerized primer CEM Unicem 2 polymerized primer polymerized primer CEM Unicem 2
primer primer primer primer

SpeedCEM RelyX Unicem 2 Control SpeedCEM RelyX Unicem 2 Control

(no primer) (no primer)
Initial sample size was n = 20 per group. Specimens that were found to Initial sample size was n = 20 per group. Specimens that were found to
have been bonded to mixed tissue (enamel and dentin) or enamel and have been bonded to mixed tissue (enamel and dentin) or enamel and
epoxy were excluded from analysis. Final sample size ranged from 16 epoxy were excluded from analysis. Final sample size ranged from 18
to 20 per group. Error bars represent the standard deviation. to 20 per group. Error bars represent the standard deviation.

Results
Table. Statistical comparison of mean shear bond strengths in Shear bond strength
all test groups. The results for the enamel bonding groups are depicted in Chart 1.
One-way ANOVA was used to compare bond strengths in primer
Group Mean (SD) and nonprimer groups. The SBS values of the primer groups were
approximately 2-3 times greater than those of the nonprimer
RU2 on dentin, photopolymerized primer 26.82 (5.62)ab groups. The air-dried SC specimens also had significantly greater
(n = 20) bond strength than the air-dried RU2 specimens within the
RU2 on dentin, air-dried primer (n = 19) 26.53 (0.88)a enamel primer groups (P < 0.001). When the enamel air-dried and
SC on enamel, photopolymerized primer 23.75 (6.75)ab photopolymerized primer groups were compared, the mean SBS
(n = 20) of the photopolymerized RU2 group was significantly higher (P <
0.001), but the 2 SC groups were equivalent to each other. There
SC on dentin, photopolymerized primer (n = 20) 23.09 (6.01)ab
was no statistically significant difference between the photopoly-
SC on dentin, air-dried primer (n = 18) 23.15 (1.36)ab merized resin cement products.
RU2 on enamel, photopolymerized primer 21.50 (5.21)ab Results for the dentin bonding groups are depicted in Chart 2.
(n = 18) One-way ANOVA was used to determine the statistical signifi-
SC on enamel, air-dried primer (n = 16) 19.34 (1.55)c cance of differences in SBS between primer and nonprimer groups.
The SBS values of all primer groups were approximately 4-6 times
RU2 on enamel, air-dried primer (n = 17) 13.75 (0.81)d greater than those of the nonprimer groups. For primer groups
Abbreviations: RU2, RelyX Unicem 2 Automix; SC, SpeedCEM. bonded to dentin, the air-dried RU2 specimens had a greater bond
Means with the same superscript letter are not significantly different strength than did the air-dried SC specimens, but the difference
(P > 0.05; post hoc Tukey test).
was not statistically significant (P = 0.17). When the dentin air-
dried and photopolymerized primer groups were compared, the

24 GENERAL DENTISTRY January/February 2020

 Chart 3. Distribution of failure modes in enamel groups. Chart 4. Distribution of failure modes in dentin groups.

20 20
18 18

16 16
14 14
Failure (No. of specimens)

Failure (No. of specimens)

12 12

10 10

8 8

6 6

4 4
2 2
0 0
SpeedCEM RelyX SpeedCEM RelyX SpeedCEM RelyX SpeedCEM RelyX SpeedCEM RelyX SpeedCEM RelyX
Unicem 2 Unicem 2 Unicem 2 Unicem 2 Unicem 2 Unicem 2

Control Air-dried primer Photopoly- Control Air-dried primer Photopoly-

merized primer merized primer

Cohesive Cohesive Adhesive Mixed Cohesive Cohesive Adhesive Mixed

in resin in tooth (adhesive-resin) in resin in tooth (adhesive-resin)

Initial sample size was n = 20 per group. Specimens that were found to Initial sample size was n = 20 per group. Specimens that were found to
have been bonded to mixed tissue (enamel and dentin) or enamel and have been bonded to mixed tissue (enamel and dentin) or enamel and
epoxy were excluded from analysis. Final sample size ranged from 16 epoxy were excluded from analysis. Final sample size ranged from 18
to 20 per group. to 20 per group.

differences were not statistically significant. Both resin cement (Chart 4). Adhesive failure dominated in the specimen groups
products followed the same pattern. without primer (94% and 83% for SC and RU2, respectively).
When all of the groups tested in the study were compared, Mixed adhesive-resin failure occurred in all of the dentin
even the weakest primer group had a significantly greater groups with primer but was more prevalent in the photopoly-
mean SBS than the strongest nonprimer group (Table). The merized primer groups. Cohesive tooth failure in dentin was
dentin primer groups had higher raw SBS values than did similar to that in enamel, occurring only in the groups with
the corresponding enamel primer groups, except for the SC photopolymerized primer. Figures 2-5 show representative
photopolymerized specimens. These differences were statisti- microphotographs of the 4 failure modes in various test groups.
cally significant except for the SC polymerized specimens. For
RU2 specimens, there was a statistically significant difference Discussion
between the enamel and dentin groups (P < 0.05). Both conventional SBS and microtensile bond strength data
have been widely reported in the literature.4,6,8-16 The present
Failure mode study used conventional SBS testing to allow simple compari-
For the enamel groups, the most common mode of failure was sons between the primer and nonprimer groups rather than pri-
adhesive failure, at 57% (Chart 3). Most of the remaining enamel marily compare the specific products. The results showed that
specimens, except the photopolymerized groups, exhibited a separate primer application significantly increased the SBSs of
cohesive failure in resin. The only enamel group in which the the tested materials to enamel and dentin, so the test hypothesis
majority of specimens exhibited cohesive resin failure consisted was accepted.
of the SC specimens prepared with air-dried primer (94%). The One of the greatest challenges in restorative dentistry is
only enamel groups that exhibited mixed adhesive-resin or to obtain a strong and durable bond at the tooth-restoration
cohesive tooth failure were those with photopolymerized primer. interface. Dental restorations rely on adhesive systems to form
For the dentin groups, mixed adhesive-resin failure pre- a micromechanical and chemical-ionic link with the tooth
dominated in the specimens with photopolymerized primer structure. Although adhesion to enamel is predictable, adhesion
for both SC and RU2 resin cements, although all groups with to dentin is challenging because of the complex composition of
primer exhibited some degree of mixed adhesive-resin failure its mineral, organic, and fluid phases.10 The newest and most

agd.org/generaldentistry 25
Comparison of 2 self-adhesive resin cements with or without a self-etching primer

Fig 2. Example of cohesive failure (in the resin) from the group Fig 3. Example of cohesive failure (in the tooth) from the group
RelyX Unicem 2 on dentin with air-dried primer. SpeedCEM on enamel with photopolymerized primer.

attractive cementation systems are, to the time-conscious prac- less technique sensitive as they are all-in-1 systems that do not
titioner, the “all-in-1” self-adhesive resin cement systems. These require additional steps to form a bond; the cement is applied
cements, based on filled polymers, are designed to adhere to directly onto the tooth structure. This method was created for
tooth structure without the requirement of a separate adhesive ease of use and to overcome the limitations of complex multi-
or etchant.17 These systems are easier to use and require less step applications, such as susceptibility to contamination and
sensitive techniques, but the bond strengths are usually not as the postoperative sensitivity that results from etching away the
strong as those demonstrated with other bonding protocols.10 dentin smear layer.12
Manufacturers have introduced multimodal universal adhe- Self-adhesive resin cements also eliminate the chemical incom-
sives to provide clinicians the choice of total-etching, selective patibility observed when dissimilar adhesive systems are used in
etching, or self-etching in single-bottle systems. Chen et al conjunction with each other.13 The concept and aim of all-in-1
performed a study using 5 universal adhesive systems in 2 bond- self-adhesive resin cements are worthwhile, but, as previously
ing modes (self-etching and etch-and-rinse).18 They concluded: noted, the bond strengths obtained are not as strong as those
“The increase in versatility of universal adhesives is not accom- exhibited by other systems.10 The limited etching potential and
panied by technological advances for overcoming the challenges superficial interaction of the cement with the dentin surface pro-
associated with previous generations of adhesives.”18 The impli- vides a lower bond strength than conventional resin cements, and
cation of their study is that altering the mode of etching via self- the smear layer left behind on the dentin surface impedes proper
adhesive bonding systems is not as effective as using a separate infiltration of the cement into dentin.12 In addition, the cement is
priming step in the bonding process. too viscous to penetrate the demineralized collagen fiber network.
De Munck et al showed that early versions of a self-adhesive The aim of the present study was to see if application of a dentin
luting material provided significantly weaker bonds than did a primer would enhance the interaction between the self-adhesive
material that had a self-etching primer in its system.19 They also resin cement and dentin. Dentin surface pretreatments with differ-
found that the self-adhesive cement obtained its most effec- ent conditioning solutions alter the chemical and structural com-
tive bond when the enamel was selectively acid etched before position of human dentin. This change in composition enhances
luting.19 Peutzfeldt et al found that 2 self-etching resin cements, the permeability and solubility characteristics that affect the
Panavia F2.0 and Multilink, resulted in higher bond strengths adhesion of materials to dentin surfaces.14 The use of nonchemical
than did the conventional etch-and-rinse resin cement Variolink dentin surface cleaning techniques, such as microparticle air abra-
II.20 Liu et al found that 3 different conventional resin cements sion (sandblasting) with aluminum oxide to remove contaminants
had significantly less water sorption and greater bond strength along the dentin-cement interface, has also been demonstrated to
than a self-adhesive cement.21 improve the bond strength of self-adhesive luting systems.23
The manufacturers of self-adhesive resin cements claim Dentin conditioning facilitates smear layer removal, but the
that no dentin pretreatment is necessary.1,2 However, this viscosity of the adhesive resin materials still hampers their pen-
claim contradicts the results of studies that show higher bond etration of dentin. Opening of the dentinal tubules permits the
strengths are achieved subsequent to pretreatment of the formation of resin tags, increasing bond strength.24 Chemical
dentin surface.11,22 Clinically, there are 3 main methods to obtain cleaning and chelating agents promote the adhesion or penetra-
a bond between tooth structure and an indirect restoration: tion of self-adhesive resin cements to create micromechanical
total-etching (etch-and-rinse), self-etching, and self-adhesive surface interlocking with dentin.14 For example, polyacrylic acid
cement systems. Self-adhesive resin cements are simpler and is a mild acid that is normally used as a conditioner before the

26 GENERAL DENTISTRY January/February 2020

Fig 4. Example of adhesive failure from the control group Fig 5. Example of mixed adhesive and resin failure from the group
SpeedCEM on dentin without primer. SpeedCEM on enamel with air-dried primer.

application of glass ionomer cements. This mild acid partially defeat the purpose of the all-in-1 self-adhesive resin cement sys-
removes the smear layer but leaves smear plugs in the tubules.25 tems; however, if a tooth preparation has inadequate retentive
Youm et al demonstrated that ethylenediaminetetraacetic acid, features, it is advisable to perform a protocol that would ensure
a calcium-chelating agent, is effective in removing the hydroxy- maximum bond strength of the tooth-restoration complex.
apatite of dental hard tissue selectively without destroying the The failure modes followed the expected pattern. One interest-
collagen matrix structure.12 Both of these examples suggest that ing observation is that the only groups that displayed cohesive
the pretreatment of the dentin surface before the application of tooth fracture were those in which the primer was photopolymer-
a self-adhesive resin cement improves bond strength. ized before placement of the adhesive resin cement. The distribu-
In a similar study by Broyles et al, 6.5% grape-seed extract, 5% tion differences were also notable. In the nonprimer groups, the
glutaraldehyde, and 25% polyacrylic acid were used as pretreat- predominant mode of failure was adhesive failure; after the simple
ments before 2 self-adhesive cements were placed on human addition of primer, the predominant modes changed to cohesive
dentin.15 For the cements tested in their study, polyacrylic acid failure in the resin and mixed adhesive-resin. This change implies
and glutaraldehyde resulted in a significant increase in micro- a much stronger attachment to the tooth, regardless of the tissue
tensile bond strength to dentin, but treatment with grape-seed tested. The light-curing step with the primer further changed the
extract alone did not.15 distribution to a combination of mixed mode and cohesive fail-
In the present study, the SBSs were greater for all the ures in the tooth. This suggests that the protocol would provide
specimens that were prepared using a primer (conditioner) in favorable results in cases where the tooth structure offers poor
addition to the self-adhesive resin cements. This finding may retention.
be explained by the following: (1) there may have been better
penetration of the dentin when the primer was used, because Conclusion
the primer is much less viscous than the all-in-1 resin cement; In this in vitro study, a separate primer application significantly
(2) the primer may be more hydrophilic than the self-adhesive increased the SBSs of self-adhesive resin cements to enamel
resin cements and have enhanced reactivity with the dentin; and and dentin. Therefore, there may be an advantage to using a
(3) there may have been a better ionic bond between the primer dedicated dentin primer to improve the clinical performance
and the calcium ions on the collagen fibers in dentin. of self-adhesive resin cements in indirect restoration of teeth,
Clearfil SE Protect primer is a self-etching primer from a especially when the preparation has poor mechanical retentive
self-etching, 2-step (sixth-generation) dental bonding system. It features. Further research is needed, however, to confirm these
contains an acidic monomer, 10-methacryloxydecyl dihydrogen findings in similar products from other manufacturers to deter-
phosphate, that can partially dissolve the smear layer and demin- mine their compatibility.
eralize the underlying dentin, which results in mild surface etch-
ing. Excellent dentin bonding with a self-etching primer system Author information
has already been demonstrated in previous laboratory studies.16,26 Dr Meharry is an assistant professor of clinical dentistry, and Dr
An interesting observation from the present study is that Mitchell is a professor, Midwestern University, College of Dental
the same primer also achieved a significantly stronger bond to Medicine-Arizona, Glendale. Drs Schwartz and Montalvo are
enamel. This result was likely due to better penetration of the former dental students, Midwestern University. Mr Mueller is a
enamel prisms, improving the micromechanical properties of current dual-degree student at the Medical University of South
the bond. The extra step of applying a self-etching primer may Carolina, Charleston.

agd.org/generaldentistry 27
Comparison of 2 self-adhesive resin cements with or without a self-etching primer

Acknowledgment 11. Pisani-Proenca J, Erhardt MC, Amaral R, Valandro LF, Bottino MA, Del Castillo-Salmeron R.
The authors gratefully acknowledge Dr Maria Teresa Pulido for Influence of different surface conditioning protocols on microtensile bond strength of self-
adhesive resin cements to dentin. J Prosthet Dent. 2011;105(4):227-235.
assistance and invaluable advice during use of the universal test- 12. Youm SH, Jung KH, Son SA, Kwon YH, Park JK. Effect of dentin pretreatment and curing
ing machine. mode on the microtensile bond strength of self-adhesive resin cements. J Adv Prosthodont.
2015;7(4):317-322.
Disclaimer 13. Rodrigues RF, Ramos CM, Francisconi PA, Borges AF. The shear bond strength of self-
adhesive resin cements to dentin and enamel: an in vitro study. J Prosthet Dent. 2015;
The authors report no conflicts of interest pertaining to any of 113(3):220-227.
the products or companies discussed in this article. 14. Egilmez F, Ergun G, Cekic-Nagas I, Vallittu PK, Lassila LV. Bond strength of self-adhesive resin
cements to dentin after antibacterial and chelating solution treatment. Acta Odontol Scand.
2013;71(1):22-31.
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28 GENERAL DENTISTRY January/February 2020

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