d e n t a l m a t e r i a l s x x x ( 2 0 0 6 ) xxx–xxx

available at www.sciencedirect.com

journal homepage: www.intl.elsevierhealth.com/journals/dema

Bonding effectiveness of adhesive luting agents to enamel

and dentin

K. Hikita a,b , B. Van Meerbeek a , J. De Munck a , T. Ikeda a,c , K. Van Landuyt a ,

T. Maida b , P. Lambrechts a , M. Peumans a,∗
a Leuven BIOMAT Research Cluster, Department of Conservative Dentistry, School of Dentistry, Oral Pathology and Maxillo-Facial
Surgery, Catholic University of Leuven, Kapucijnenvoer 7, 3000 Leuven, Belgium
b Institute of Medical Science, Health Sciences University of Hokkaido, 2-5 Ainosato, Kita-ku, Sapporo 002-8072, Japan
c Section of Cariology, Operative Dentistry and Endodontology, Department of Oral Health Science, Hokkaido University Graduate School

of Dental Medicine, Kita 13 Nishi 7, Kita-ku, Sapporo 060-8586, Japan

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

Article history: Objectives. The bonding effectiveness of five adhesive luting agents to enamel and dentin
Received 18 July 2005 using different application procedures was determined using a micro-tensile bond strength
Received in revised form protocol (␮TBS).
1 December 2005 Methods. Enamel/dentin surfaces of human third molars were flattened using a high-speed
Accepted 1 December 2005 diamond bur. Composite resin blocks (Paradigm, 3 M ESPE) were luted using either Linkmax
(LM; GC), Nexus 2 (NX; Kerr), Panavia F (PN; Kuraray), RelyX Unicem (UN; 3M ESPE) or Vari-
olink II (VL; Ivoclar-Vivadent), strictly following manufacturers’ instructions. For some luting
Keywords: agents, modified application procedures were also tested, resulting in four other experimen-
Adhesion tal groups: Prompt L-Pop + RelyX Unicem (PLP + UN; 3 M ESPE), Scotchbond Etchant + RelyX
Resin cement Unicem (SE + UN; 3 M ESPE), Optibond Solo Plus Activator + Nexus 2 (ACT + NX; Kerr) and K-
Micro-tensile bond strength Etchant gel + Panavia-F (KE + P; Kuraray). The experimental groups were classified according
Indirect resin composite to the adhesive approach in self-adhesive (UN), etch-and-rinse (ACT + NX, NX, KE + P, SE + UN
CAD/CAM and VL when bonded to enamel) and self-etch adhesive luting agents (LM, PLP + UN, PN and
VL when bonded to dentin). The specimens were stored for 24 h in distilled water at 37 ◦ C
prior to ␮TBS testing. The Kruskal–Wallis test was used to determine pairwise statistical
differences (p < 0.05) in ␮TBS between the experimental groups.
Results. When bonded to enamel, ACT + NX (15 MPa) and UN (19.6 MPa) scored significantly
lower than VL (49.3 MPa), LM (49.2 MPa), PN (35.4 MPa) and SE + UN (35.2 MPa), while PLP + UN
(23.5 MPa) showed a significantly lower ␮TBS than VL (49.3 MPa) and LM (49.2 MPa). No signif-
icant differences were noticed between VL (49.3 MPa), LM (49.2 MPa), NX (37.9 MPa), KE + PN
(38.8 MPa), PN (35.4 MPa) and SE + UN (35.2 MPa). Regarding the bonding effectiveness to
dentin, all luting agents bonded equally effectively (UN: 15.9 MPa; LM: 15.4 MPa; PN: 17.5 MPa;
NX: 22.3 MPa), except VL (1.1 MPa), SE + UN (5.9 MPa) and ACT + NX (13.2 MPa). VL revealed an
exceptionally high number of pre-testing failures, most likely due to a combined effect of
not having cured the adhesive separately and an insufficiently light-cured luting agent.
Significance. Following a correct application procedure, the etch-and-rinse, self-etch and self-
adhesive luting agents are equally effective in bonding to enamel and dentin. Several factors

∗
Corresponding author. Tel.: +32 16 33 27 44; fax: +32 16 33 27 52.
E-mail address: marleen.peumans@med.kuleuven.ac.be (M. Peumans).
0109-5641/$ – see front matter © 2005 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.
doi:10.1016/j.dental.2005.12.002

DENTAL-892; No. of Pages 10

2 d e n t a l m a t e r i a l s x x x ( 2 0 0 6 ) xxx–xxx

negatively influenced bond strength such as bonding RelyX Unicem to enamel without prior
phosphoric acid etching; no separate light-curing of a light-polymerizable adhesive prior
to cementation, use of a light-polymerizing adhesive converted into a dual-polymerizing
adhesive, and use of a dual-cure luting agent with a low auto-polymerizable potential.
© 2005 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

1. Introduction
Indirect adhesive procedures constitute a substantial por-
tion of contemporary esthetic restorative treatments. Tooth-
colored inlays, onlays, veneers and crowns are now routinely
bonded to the tooth substrate via the use of adhesive resin
cements [1–3]. Adhesive resin cements have the ability to
bond to both tooth structure and restoration. The integration
produces reinforcement of both structures [4,5], and reduces
microleakage at the restoration-tooth interface, postoperative
sensitivity, marginal staining and recurrent caries.
Tooth-colored restorations can be constructed in a rela-
tively simple way by CAD–CAM techniques using prefabricated
ceramic or composite blocks manufactured under controlled
conditions. Indirect composite restorations are now more rou-
tinely used because composite blocks show some advantages
over ceramic blocks as these have easier finishing and pol-
ishing, kinder to the natural dentition with regard to wear
and easier to make add-on adjustment. In addition, higher
bond strengths to pre-treated composite compared with pre-
treated ceramic are reported in vitro [6], probably due to a more
compliant situation as the modulus of elasticity of the luting
agent and the composite are in the same range. Consequently,
several in vitro studies found a more uniform stress distribu-
tion throughout teeth restored with indirect composite inlays,
compared to ceramic inlays [7,8].
Besides the advantages of the indirect composite restora-
tion, bonding to tooth structure is still a challenging matter,
as the indirect restorative procedure will double the adhesive
interfaces. One interface is at the tooth structure and the other
at the fitting surface of the restoration. In order to establish a
strong and durable bond, which is necessary for the biome-
chanical aspect of the tooth-restoration system, appropriate
treatment of the respective surfaces is crucial.
Adhesion of resin cement to processed composites has
traditionally been difficult to achieve [9]. Roughening the
composite surface by bur or by sandblasting, followed by
silanization has been recommended as a predictable means
for enhancing retention between resin cements and the indi-
rect composite restoration [6,10].
At the tooth surface, an adhesive system is used to bond
the luting agent to the tooth substrate. Currently, all adhesives
are categorized as either etch-and-rinse or self-etch adhesives
[11]. A multi-step application technique is time consuming
and rather technique sensitive, and consequently may com-
promise bonding effectiveness [12]. Recently, a self-adhesive
universal resin cement without surface pre-treatment has
been introduced (RelyX Unicem; 3 M ESPE, Seefeld, Germany).
This self-adhesive resin cement is based on a new monomer,
filler and initiation technology. The manufacturer purports
that the organic matrix consists of newly developed mul-
tifunctional phosphoric acid methacrylates. The phospho-
ric acidic methacrylates can react with the basic fillers in
the luting cement and the hydroxyapatite of the hard tooth
tissue.
Several in vitro studies reported the bond strength of differ-
ent adhesive systems used in combination with a luting com-
posite to both enamel and dentin [13–17]. Little information,
however, is available in the literature with regard to the bond
strength of the complete tooth/indirect restoration complex
using different luting composites categorized by their adhe-
sive system. The purpose of this study was to assess the bond-
ing effectiveness of five adhesive luting agents to enamel and
dentin with different application procedures using a standard
micro-tensile bond strength (␮TBS) test set-up. The hypothe-
sis tested in this study was that there were no differences in
bonding effectiveness between etch-and-rinse, self-etch and
self-adhesive luting agents.
2. Materials and methods
Forty-two non-carious human third molars (gathered follow-
ing informed consent, approved by the Commission for Medi-
cal Ethics of the Catholic University of Leuven) were stored in
0.5% chloramine in water at 4 ◦ C and used within 1 month after
extraction. The teeth were randomly divided into 17 experi-
mental groups.
Specimen preparation is schematically shown in Fig. 1.
Table 1 shows the list of adhesive luting agents with their
respective application procedures investigated. The general
composition of the adhesive luting agents is described in
Table 2.
3. Enamel specimen preparation for ␮TBS
Lingual and/or buccal enamel was flattened using a high-
speed diamond bur (842, Komet, Lemgo, Germany), mounted
in a MicroSpecimen Former (University of Iowa, Iowa City,
IA, USA). Prior to cementing procedures CAD/CAM composite
blocks (max. 7 mm thick; Paradigm MZ100, 3 M ESPE, St. Paul,
MN, USA) were cut using a low-speed diamond saw (Isomet
1000, Buehler, Lake Bluff, IL, USA) to obtain a standard sur-
face roughness. The bonding surface was prepared according
to the manufacturer’s instructions for the respective cement.
For some luting agents an additional experimental group was
made by modifying the adhesive bonding procedure. In total,
nine experimental groups were made, classified according to
the category of adhesive in etch-and rinse, self-etch and self-
adhesive luting agents (Table 1).
Next, the resin cement was applied on the enamel sur-
face after surface treatment according to the manufacturer’s
instructions. The CAD/CAM composite block was pressed on
the cement using light pressure, after which excess cement
was removed. Light-curing was performed from four parallel
 d e n t a l m a t e r i a l s x x x ( 2 0 0 6 ) xxx–xxx 3

Fig. 1 – Schematic drawing illustrating the study set-up and specimen preparation.

directions along the cement interface using an Optilux 500
(Demetron/Kerr, Danbury, CT, USA) device with a light output
not less than 550 mW/cm2 . At each moment during specimen
processing, care was taken to prevent dehydration of the spec-
imens.
4. Dentin specimen preparation for ␮TBS
The occlusal third of the molars was removed using the Isomet
slow-speed diamond saw. Dentin surfaces were controlled for
absence of enamel and/or pulp tissue using a stereomicro-
scope (Wild M5A, Heerbrugg, Switzerland). The teeth were
mounted in a chuck and a standard smear layer was produced
by removing a thin layer of the surface using a high-speed
medium grit (100 ␮m) diamond bur (842, Komet) mounted in
the MicroSpecimen Former. The cements were subsequently
applied following the methodology described by the manufac-
turer. Similar to the enamel specimens, a modified application
procedure was added for some luting agents. In total, eight
experimental groups were prepared for testing (Table 1).
face (N) at the time of fracture by the bond area (mm2 ). When
specimens failed before actual testing, the ␮TBS was deter-
mined from the specimens that survived specimen processing
with an explicit note of the number of pre-testing failures.
For the dentin and the enamel side, Kruskal–Wallis test was
used to determine pairwise statistical differences (p < 0.05) in
␮TBS between the experimental groups. All statistics were
performed using the Statistica software package (StaSoft, OK,
USA).
The mode of failure was determined at a magnification of
50× using a stereomicroscope (Wild M5A).
6. Results
The mean ␮TBS values are graphically presented per experi-
mental group in box-whisker plots in Fig. 2 (enamel) and Fig. 3
(dentin). Statistically significant differences are mentioned in
Table 3. Figs. 4 and 5 show a graphical presentation of propor-
tional prevalence of failure modes for all experimental groups
when bonded to enamel (Fig. 4) and dentin (Fig. 5).

5. ␮TBS testing

After 24 h of water storage, the teeth were sectioned perpen-

dicular to the adhesive-tooth interface using the Isomet saw
to obtain rectangular sticks of about 2 mm × 2 mm width and
8–9 mm long. Specimens were trimmed at the biomaterial-
tooth surface to a cylindrical hourglass shape with a diameter
of about 1.2 mm using the MicroSpecimen Former and fine
cylindrical diamond burs (Ø = 1.2 mm, 835KREF, Komet, Lemgo,
Germany) under continuous air/water spray. Next, the cross-
sectional diameter was precisely (accuracy = 0.001 mm) mea-
sured using a precision measuring instrument transformed
from an x–y multi-purpose modular microscope (Leitz, Wet-
zlar, Germany). Specimens were then fixed to Ciucchi’s jig (fix- Fig. 2 – Box plot of enamel ␮TBS results. The box
ation height = 4–6 mm) with cyano-acrylate glue (Model Repair represents the spreading of the data between the first and
II Blue, Dentsply-Sankin, Ohtawara, Japan) and stressed at a third quartile. The central vertical line represents the
crosshead speed of 1 mm/min until failure in a LRX mate- median. The whiskers extend to the minimum and
rial testing device (LRX, Lloyd, Hampshire, UK). The ␮TBS was maximum value measured. ptf/n = number of pre-testing
expressed in MPa, as derived from dividing the imposed sur- failures/total specimen number.
4 d e n t a l m a t e r i a l s x x x ( 2 0 0 6 ) xxx–xxx

Table 1 – List of luting agents and their respective adhesive application procedures
Code Product name Manufacturer Enamel/dentin pre- Composite pre- Luting agent mixing
treatment treatment

Self-adhesive
UN RelyX Unicem 3 M ESPE, No pre-treatment No pre-treatment Mix the capsule for 15 min
Seefeld, (Rotomix, 3 M ESPE), apply
Germany on surface; lute resin
block, light cure for 20 min
from each side

Self-etch
LM Linkmax GC, Tokyo, Mix one drop of each Apply GC Etchant liquid for Mix A-paste and B-paste
Japan primer liquids EP-A and 30 s, rinse, air dry, mix one for 10–20 s, light cure for
EP-B for 5 s, apply, air dry drop of each Ceramic 20 s from each side
after 30 s Primers A and B for 5 s,
apply, air dry
PLP + UN Prompt L-Pop 3 M ESPE, Apply Prompt L-Pop, No pre-treatment Mix the capsule for 15 s
+ RelyX Unicem Seefeld, rubbing for 15 s, air blow to (Rotomix, 3 M ESPE), apply
Germany thin film, light cure for 10 s on surface; lute resin
block, light cure for 20 s
from each side
PN Panavia-F Kuraray, Mix one drop of each ED Apply K-Etchant gel for 5 s, Mix universal and catalyst
Osaka, Japan Primer liquids A and B for rinse, air dry, mix one drop paste for 20 s, light cure
5 s, apply, air dry gently of each Cleafil SE Primer for 20 s from each side
after 60 s and Porcelain Bond after removal excess
Activator for 5 s, apply cement, apply oxyguard
for 3 min
VLa Variolink II Ivoclar- Apply Total Etch (37% Apply Monobond-S for 60 s, Mix base and catalyst
Vivadent, phosphoric acid) only on air dry, apply Heliobond paste, light cure for 20 s
Schaan, enamel for 15 s, rinse, air from each side
Liechtenstein dry, apply Syntac primer
for 15 s, air dry, apply
Syntac adhesive for 10 s,
air dry, apply Heliobond
Etch-and-rinse
ACT + NX Optibond Solo Plus Kerr, Orange, Apply Kerr Gel Etchant Apply Kerr Gel Etchant for Mix base and catalyst
Activator + Nexus 2 CA, USA (35% phosphoric acid) for 15 s, rinse, air dry, apply paste for 10–20 s, light
15 s, rinse, air dry, mix one Silane Primer, air dry cure for 40 s from each
drop of Optibond Solo Plus side
and Optibond Solo Plus
Activator for 3 s, apply for
15 s, air dry
NX Nexus 2 Kerr, Orange, Apply Kerr Gel Etchant Apply Kerr Gel Etchant for Mix base and catalyst
CA, USA (37% phosphoric acid) for 15 s, rinse, air dry, apply paste for 10–20 s, light
15 s, rinse, air dry, apply Silane Primer, air dry cure for 40 s from each
Optibond Solo Plus for 15 s, side
air dry, light cure for 20 s
KE + PNb K-Etchant Kuraray, Apply K-Etchant gel (40% Apply K-Etchant gel for 5 s, Mix universal and catalyst
gel + Panavia-F Osaka, Japan phosphoric acid) on rinse, air dry, mix one drop paste for 20 s, light cure
enamel for 10 s, rinse, air of each Cleafil SE Primer for 20 s from each side
dry. Mix one drop of each and Porcelain Bond after removal excess
ED Primer liquids A and B Activator for 5 s, apply, air cement, apply oxyguard
for 5 s, apply, air dry gently blow, polymerization for for 3 min
after 60 s 10 s
SE + UN Scotchbond 3 M ESPE, Apply Scotchbond Etchant No pre-treatment Mix the capsule for 15 s
Etchant + RelyX Seefeld, (35% phosphoric acid) for (Rotomix, 3 M ESPE), apply
Unicem Germany 15 s, rinse, air dry on surface, lute resin
block, light cure for 20 s
from each side

a
VL: self-etch adhesive that requires selective etching of enamel with phosphoric acid.
b
Condition ‘KE + PN’ was not applied for dentin.
 d e n t a l m a t e r i a l s x x x ( 2 0 0 6 ) xxx–xxx 5

Table 2 – General composition of adhesive luting agents tested in this study

Material (manufacturer) Composition Batch no.

Linkmax (GC Corp., Tokyo, Japan) Primer A: 4-META, HEMA, dimethacrylate, water, ethanol 301101
Primer B: ethanol, initiator 301101
Paste A: fluoroaluminosilicate glass, urethane dimethacrylate, silica, 301091
photo-initiator
Paste B: fluoroaluminosilicate glass, urethane dimethacrylate, silica, 301091
photo-initiator
Nexus 2 (Kerr Co., Orange, CA, USA) Optibond Solo Plus: ethanol, Bis-GMA, barium aluminoborosilicate glass, silica, 203D20
sodium hexafluorosilicate
Optibond Solo Plus Activator: ethanol, Bis-GMA, sodium benzenesulfinate 204A61
Base: Bis-GMA, camphoroquinon, barium aluminoborosilicate glass 111787
Catalyst: Bis-GMA, teriethylene glycol dimethacrylate, barium 201754
aluminoborosilicate glass
Panavia F (Kuraray Medical Inc., Primer A: HEMA, 10-MDP, 5-NMSA, water, accelerator 00108B
Tokyo, Japan)
Primer B: 5-NMSA, water, sodium benzene 00115B
Paste A: 10-MDP, 5-NMSA, silica, dimethacrylate monomer, photo-initiator, 00124A
accelerator
Paste B: barium glass, sodium fluoride, dimethacrylate monomer, BPO 00046A
K-Etchant: 40% phosphoric acid, thicknener

RelyX Unicem (3 M ESPE, Seefeld, Powder: glass powder, silica, calcium hydroxide, pigment, substituted 001/0001
Germany) pyrimidine, peroxy compound, initiator
Liquid: methacrylated phosphoric ester, dimethacrylate, acetate, stabilizer,
initiator
Scotchbond Etchant: 35% phosphoric acid, silica thicknener 001/0001

Prompt L-Pop (3M ESPE, Seefeld, di-HEMA-phosphate, complex fluoride, water

Germany)

Variolink II (Ivoclar-Vivadent,
Schaan, Liechtenstein)
Syntac primer: maleic acid, TEGDMA, water, acetone D58446
Syntac adhesive: maleic acid, TEGDMA, glutaraldehyde, water D59471
Heliobond: Bis-GMA, TEGDMA D58236
Paste A: Bis-GMA, urethane dimethacrylate, TEGDMA, inorganic filler, D61246
ytterbium trifluoride, initiator, stabilizer
Paste B: Bis-GMA, urethane dimethacrylate, TEGDMA, inorganic filler, D61049
ytterbium trifluoride, benzoyl peroxide, stabilizer

At the enamel, the lowest ␮TBS values were measured
for ACT + NX (15 MPa), UN (19.6 MPa) and PLP + UN (23.5 MPa)
with no significant differences between these three groups.
The highest ␮TBS values were obtained with VL (49.3 MPa)
and LM (49.2 MPa), while NX (37.9 MPa), PN (35.4 MPa), KE + PN
(38.8 MPa) and SE + UN (35.2 MPa) scored in between. No statis-
tically significant differences were noted between these latter
six experimental groups. ACT + NX and UN scored significantly
lower than LM, PN, SE + UN and VL, while for PLP + UN the dif-
ference was only significant with LM and VL.
Failure analysis of the ␮TBS fracture surfaces demon-
strated that when bonded to enamel most UN specimens

Table 3 – P-values from pairwise statistical comparisons (Kruskal–Wallis test)

Dentin Enamel

UN NX ACT + NX KE + PN SE + UN VL LM PN PLP + UN
****
UN 0.0628 0.9171 0.13 0.0188 0.0005 0.0005 0.0052 0.9539
****
NX 0.7452 0.992 >0.9999 >0.9999 0.7094 0.7062 0.9997 0.3396
****
ACT + NX 0.9118 0.2109 0.0777 0.0178 0.0021 0.0022 0.0086 0.6193
** ** ** ****
KE + PN 0.9994 0.8815 0.783 0.9999 0.425
** ****
SE + UN 0.0201 0.0013 0.4277 0.1133 0.1327 >0.9999 0.141
** ****
VL 0.003 0.0006 0.029 0.0078 >0.9999 0.0574 0.0015
** ****
LM >0.9999 0.8695 0.8326 0.0408 0.002 0.0612 0.0018
** ****
PN 0.9984 0.9655 0.5176 0.0019 0.0009 >0.9999 0.0752
** ****
PLP + UN 0.0362 0.9997 0.0017 0.0008 0.0004 0.4083 0.3663

In the right upper half of the table (above asterisks), p-values of comparisons between enamel ␮TBS are presented. In the left lower half of
the table (below asterisks), p-values of comparisons between dentin ␮TBS are presented. p-Values underlined with an uninterrupted line are
smaller than 0.05 and thus indicate significant difference; p-values with an interrupted line represent nearly statistically significant difference.
6 d e n t a l m a t e r i a l s x x x ( 2 0 0 6 ) xxx–xxx

Fig. 3 – Box plot of dentin ␮TBS results. The box represents

the spreading of the data between the first and third
quartile. The central vertical line represents the median.
The whiskers extend to the minimum and maximum value
measured. ptf/n = number of pre-testing failures/total
specimen number.

(78.6%) showed adhesive failures at the luting-enamel inter-

face. For LM, cohesive failures in enamel were the predom-
inant type of failure (78.6%), while the ACT + NX specimens
failed mainly (70%) cohesively in the luting agent. For the other
luting agents (NX, PN, VL, KE + PN and SE + UN), the failure pat-
tern was a mixture of several types of failure.
Regarding the bonding effectiveness to dentin, all lut-
Fig. 5 – Graphical presentation of proportional prevalence
ing agents bonded equally effectively (LM: 15.4 MPa; NX:
of fracture modes for all experimental groups when bonded
22.3 MPa; PN: 17.5 MPa; UN: 15.9 MPa), except VL (1.1 MPa),
to dentin.
SE + UN (5.9 MPa) and ACT + NX (13.2 MPa). VL revealed an
exceptionally high pre-testing failure number (10/12). The

highest bond strengths were measured for NX (22.3 MPa),

PLP + UN (22.2 MPa), while LM (15.4 MPa), PN (17.5 MPa) and UN
(15.9 MPa) scored in between. Among these latter five groups,
no significant differences were noticed, except for PLP + UN,
which scored significantly higher than UN.
The bond strength of VL to dentin was significantly lower
than for all other experimental groups, and etching of dentin
with phosphoric acid prior to application of RelyX Unicem
(SE + UN) resulted in a significantly lower bond strength, as
compared to LM, NX, PN, UN and PLP + UN.
Concerning the failure modes at the dentin, LM (90%),
PN (80%) and SE + UN (100%) specimens failed predominantly
adhesively between dentin substrate and luting agent, while
in the NX group, most specimens failed (81.8%) adhesively at
the luting-Paradigm interface. Next, PLP + UN and ACT + NX
showed a 100% and 70% (respectively) cohesive failure in
the luting agent. Finally, application of UN and VL to dentin
resulted in a mixture of failures at the luting-dentin interface.

7. Discussion

Indirect composite restorations are preferred to direct com-

Fig. 4 – Graphical presentation of proportional prevalence posite restorations when restoring large tooth defects because
of fracture modes for all experimental groups when bonded of several advantages such as better marginal adaptation
to enamel. and anatomic form, more resistance to wear, increased frac-
 d e n t a l m a t e r i a l s x x x ( 2 0 0 6 ) xxx–xxx
ture resistance and more control of polymerization shrink-
age [18–20]. The longevity of the indirect composite restora-
tion is influenced by the physico-mechanical properties of the
restoration and luting agent, but mainly by the bonding effec-
tiveness at the tooth/indirect restoration complex [21]. The
purpose of this in vitro study was to evaluate the bonding
effectiveness of this complex using five luting composites in
combination with different application procedures.
The luting cements tested in this study were all dual-cure
resin cements. Their polymerization is initiated by light and
chemically and are therefore the materials of choice to lute
indirect tooth-colored restorations with a thickness >3 mm
[22,23]. When these dual-cure resin cements are light polymer-
ized, the highest conversion rate is reached [23], with a conse-
quent increase in the physico-mechanical properties [24–26].
Paradigm CAD–CAM composite blocks with a thickness of
7 mm were used in this study as a standard indirect compos-
ite restoration. The kind of surface treatment is important to
strongly bond to such CAD/CAM generated composite mate-
rial [27]. The Paradigm surface in the present study was treated
according to the instructions of the respective manufacturer
of each luting composite tested. For most luting agents (NX,
PN and LM), a standard surface roughness was produced by
cutting the blocks with a low speed diamond saw, followed
by etching with phosphoric acid and silanization, as it is also
recommended by several authors [6,10]. The most essential
contribution to this bond is suggested to result from the silane
treatment [17,28]. Using Variolink II (Ivoclar-Vivadent, Schaan,
Liechtenstein), the composite surface was silanized, followed
by application and polymerization of an adhesive resin. The
additional application of the adhesive resin as a surface wet-
ting agent may have positively influenced the bond strength
of the resin cement to the Paradigm composite surface [6,17].
Among all luting agents tested, RelyX Unicem was the only
one that did not require surface treatment according to the
instructions of the manufacturer. However, no information is
available in the literature with regard to the effect of surface
treatment of CAD/CAM composite blocks on the bond strength
of this luting cement.
As the most important factor determining the bonding
effectiveness of the tooth/restoration complex is the adhesive
system [21], the luting cements were categorized according
to their adhesive system as etch-and-rinse (NX, ACT + NX,
SE + UN, KE + PN and VL when bonded to enamel), self-etch
(LM, PN, PLP + UN and VL when bonded to dentin) and self-
adhesive (UN) luting agents.
Regarding the bonding effectiveness to enamel, the low-
est scores were measured for the three experimental groups
ACT + NX, UN and UN + PLP. The specimens of the ACT + NX
group exhibited the lowest enamel bond strength with 4 out
of 14 specimens having failed prior to testing. A low bond
strength was also observed at the dentin side. In both exper-
imental groups the light-cure adhesive Optibond Solo Plus
(Kerr, Orange, CA, USA) was converted into a dual-cure adhe-
sive by mixing Optibond Solo Plus with Optibond Solo Plus
Activator (Kerr), which obviously also decreased the concen-
tration of photo-initiator. As the dual-cure adhesive was not
separately light-cured, the polymerization of the adhesive
(at the deepest parts underneath the Paradigm block) relied
mainly on chemical curing. Several in vitro studies noticed a
7
lower conversion rate for dual-cure resin cements after chem-
ical curing compared to when they were exposed to light as
well [29–31]. This must also have been the case for the dual-
cure adhesive in the present study, which showed low bond
strength to both enamel and dentin. A similarly low bond
strength to dentin was also reported by other authors for the
previous dual-cure version of the Nexus adhesive [15,17]. In
the laboratory study of Mota et al., the failure pattern was
predominantly ‘adhesive’ at the dentin side [15]. This was
in contrast with the results of the present study, where the
fracture mode at both enamel and dentin sides was predom-
inantly (70%) ‘cohesive’ in the luting agent. It is not known if
the dual cure version of Optibond Solo Plus may have affected
the polymerization of the Nexus 2 luting agent (Kerr).
The second experimental group which optimally bonded
less to enamel was the self-adhesive luting cement (UN).
RelyX Unicem showed mainly adhesive failures (78.6%) at the
enamel/cement interface. Morphological SEM and TEM eval-
uation of the interface by De Munck et al. [32] revealed that
RelyX Unicem only superficially interacted with the enamel.
The limited micro-mechanical retention might be responsi-
ble for the relatively low bond strength to enamel measured
in this study. Indeed, acid etching of enamel with phospho-
ric acid prior to application of the luting cement significantly
increased its enamel bond strength. Also pre-treatment of the
enamel with a strong one-step self-etch adhesive, Prompt L-
Pop (3 M ESPE, Seefeld, Germany), increased the bond strength
slightly but not significantly. Although TEM and SEM photomi-
crographs of an enamel surface treated with Prompt L-Pop
showed an etching pattern resembling that of the etch-and-
rinse adhesives [33–35], several in vitro studies reported a
somewhat lower bond strength of Prompt L-Pop to enamel as
compared to that of etch-and-rinse adhesives [33–36]. These
results are in accordance with the results of the present study.
The highest bond strengths to enamel were obtained with
PN, LM, SE + UN, KE + PN, NX and VL with no significant differ-
ences amongst these six groups. So, the results of this study
indicate that the etch-and-rinse (NX, KE + PN, SE + UN and VL)
and self-etch approaches (LM and PN) were equally effective
in bonding to enamel (except for the two experimental groups
mentioned above: ACT + NX and UN). The self-etch adhesive
luting cements LM and PN are mild one-step self-etch adhe-
sives, producing a much less micro-retentive etching pattern
on enamel as compared to that produced by etch-and-rinse
adhesives [37–40]. Nevertheless, several laboratory studies
demonstrated relatively high initial bond strengths to instru-
mented enamel using mild self-etch adhesives [33,41–43].
Some authors found a lower bonding effectiveness when com-
pared to etch-and-rinse adhesives [39,41,43,44], while others
reported a similar bonding effectiveness [40,42,45,46] as in the
present study. This was clearly demonstrated for Panavia-F
(Kuraray, Osaka, Japan), showing similar bond strengths with
(KE + PN) and without (PN) prior enamel phosphoric acid etch-
ing. Both experimental groups (PN and KE + PN) showed a mix-
ture of several types of failure. Using Linkmax (GC, Tokyo,
Japan) (LM), most of the failures after micro-tensile testing
were cohesive in enamel, confirming the relatively strong
bond of LM to enamel.
One has to take into account that the bond strength values
measured in this study are the values after 24 h of water stor-
8 d e n t a l m a t e r i a l s x x x ( 2 0 0 6 ) xxx–xxx
age. An in vitro study of Frankenberger and Tay [47] reported a
significant decrease in gap-free margins at the enamel margin
of Class-II composite restorations placed using a one-step self-
etch adhesive after thermo-mechanical fatigue loading. This
was probably attributed to the fact that all-in-one adhesives
are more susceptible to water sorption and behave as perme-
able membranes after polymerization [48,49]. Future studies
need to find out how well one-step self-etch adhesive luting
agents resist durability testing.
At the dentin, the lowest bond strength was measured for
VL with 10 out of 12 specimens having failed prior to test-
ing. The first reason for this very low bond strength is that
the adhesive was not separately light-cured before applica-
tion of the luting cement. Indeed, additional light-curing of
the adhesive Syntac and Heliobond (Ivoclar-Vivadent, Schaan,
Liechtenstein) prior to cementation has been demonstrated to
increase the dentin bond strength [50] as well as to improve the
marginal adaptation to dentin or to the restoration [51]. How-
ever, separately light-curing the bonding agent may increase
resin thickness and thus affect accurate fit of the restoration
in the prepared cavity [50]. That might be the reason why Var-
iolink/Syntac is recommended to lute inlay or crown restora-
tions without prior polymerization of the bonding layer.
Several authors recommended a dual-bonding technique
as an alternative to light-curing the adhesive before appli-
cation of the luting agent without interfering with the fit of
the restoration [14,52,53]. This technique involves the appli-
cation and polymerization of the adhesive to freshly prepared
dentin immediately after cavity preparation before taking the
impression. It was shown to considerably increase the bond
strength values. However, no long-term clinical data for tooth-
colored inlays bonded with this technique are available at this
moment.
A second reason for the unfavourable low bond strength of
VL to dentin is the 7 mm thickness of the Paradigm blocks. The
light intensity is drastically reduced when light is transmit-
ted through a 7 mm thick composite block, so that the luting
cement must rely almost completely on its self-cure capability.
In vitro studies reported a lower auto-polymerizable poten-
tial for Variolink II, as compared with several other dual-cure
cements [23–25]. This leads to an insufficient conversion rate
when used in a self-cure mode. Indeed, Variolink II appears
to require enough light to obtain an adequate polymerization
efficiency rate and bond strength, as was confirmed by addi-
tional testing using 3 mm thick Paradigm composite blocks
(unpublished data).
Acid etching prior to application of RelyX Unicem was
detrimental for effective dentin bonding. The bond strength
of RelyX Unicem to phosphoric acid-etched dentin was sig-
nificantly lower than for PN, LM, NX, PLP + UN and VL. This
must be attributed to inadequate infiltration of the thick
and compact collagen mesh (exposed by phosphoric acid) by
the viscous cement, as was previously revealed by Fe-SEM
and TEM [32]. A weak layer of hydroxyapatite-depleted colla-
gen remained in between RelyX Unicem and the unaffected
dentin, and explains the 100% adhesive failure rate in this
experimental group. Application of RelyX Unicem without pre-
treatment (as recommended by the manufacturer), however,
gives a significantly higher bond strength to dentin. The bond-
ing mechanism of this cement is not yet completely under-
stood, but differs from that obtained with self-etch adhe-
sives as no distinct demineralization and hybridization was
observed during TEM morphological interface examination
[32,54].
Pre-treatment of dentin with the strong one-step self-
etch adhesive Prompt L-Pop further significantly increased the
bond strength to dentin (PLP + UN). The bond strength was
not significantly different from that of LM, PN and NX. On the
contrary, many laboratory [36,55,56] and (short-term) clinical
studies [57–59] noticed an inefficient bonding effectiveness for
this particular adhesive. Several explanations such as incom-
plete wetting and an insufficiently thick adhesive layer, phase
separation between hydrophilic and hydrophobic ingredients,
resultant sensitivity to hydrolysis and inhibition of polymer-
ization of the restorative composite on top due to the high
acidity of Prompt L-Pop at the oxygen-inhibited layer, have
been advanced to explain this inconsistent bonding perfor-
mance of Prompt L-Pop to dentin. The additional application of
a luting composite (on top of Prompt L-Pop) may have served as
a conventional hydrophobic resin layer removing several of the
above-mentioned explanations for the relatively low bonding
effectiveness of the sole use of Prompt L-Pop, thereby explain-
ing the more favourable bonding effectiveness registered in
this study. Nevertheless, the 100% cohesive failure rate in the
luting cement might still be due to incomplete polymerization
of the luting cement, possibly affected by the high acidity of
Prompt L-Pop.
The highest bond strength to dentin was obtained with
the light-curing adhesive Optibond Solo Plus in combina-
tion with Nexus 2 (NX). Most failures (81.8%) in this group
were adhesive at the luting-Paradigm interface, indicating a
high bond strength of the luting cement to dentin. No sig-
nificant differences in bond strengths to dentin were noticed
between this etch-and-rinse luting composite (NX), the self-
etch luting agents (LM, PN and PLP + UN) and the self-adhesive
cement (UN). Nevertheless, their failure modes were differ-
ent. All specimens using the self-etch adhesive luting agents
PN and LM showed an adhesive failure at the luting-dentin
interface. This failure mode was also observed in several other
in vitro investigations [12,13,16,60] and was explained by the
fact that one-step self-etch adhesives, because of their higher
concentration of hydrophilic monomers and the lack of the
subsequent application of a more hydrophobic resin coating,
behave as semi-permeable membranes after polymerization
[61]. In addition, as relatively less hydrophobic monomers are
available on the tooth surface after application of a one-step
self-etch adhesive, the mechanical strength of the adhesive
decreases and impairs the bond strength [35,62]. Covering the
primed dentin with a more hydrophobic adhesive layer, that
is separately light-cured before cementation, increases the
bond strength [13,14,16,63–65] and decreases the presence of
nanoleakage within the hybrid layer [13].
We may conclude that the results of the study support the
tested hypothesis that the etch-and-rinse, self-etch and self-
adhesive luting agents showed an equal bond strength to both
enamel and dentin, but only on the condition that a correct
adhesive procedure was carried out.
Finally, discussing the clinical implications of the results of
this study, one must bear in mind that the testing procedure
is more simplified than an in vivo situation. The composite
 dental materials
block was bonded to a flat surface, which represents a situa-
tion of maximum compliance as there is unrestricted shrink-
age strain (i.e. free curing contraction) of the resin cement. In
clinical circumstances, when placing an indirect inlay, onlay
or crown, the configuration factor will be higher, which may
impair the bonding effectiveness of the luting agent [37,66].
Therefore, further studies are needed to determine the effect
of polymerization contraction stress on the bonding effective-
ness of indirect restorations in prepared cavities. In addition,
as the durability of the bond greatly determines the longevity
of the restoration, there is certainly a need to test the bond
durability of adhesive luting agents in vitro and in vivo.
8. Conclusions
An adequate bonding effectiveness to tooth structure can be
obtained after 24 h of water storage with all luting agents
tested, on the condition that a correct adhesive procedure
was carried out. Some factors negatively influenced the bond-
ing effectiveness; these are: (1) not separately light-curing the
adhesive before luting; (2) use of a light-cure adhesive con-
verted into a dual-cure version; (3) use of a dual-cure luting
agent with low auto-polymerizable potential; (4) acid etching
dentin with phosphoric acid prior to the use of RelyX Unicem;
(5) bonding of RelyX Unicem to enamel without prior phospho-
ric acid etching. Taking these factors into account, the etch-
and-rinse, self-etch and self-adhesive luting cements tested in
this study are equally effective to bond to enamel and dentin,
at least in the short term.
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