THE JOURNAL OF

ADHESIVE
DENTISTRY

VOLUME 9 • SUPPLEMENT 2

2007
 All inclusive

bondi Etch Bond Easy Bond Fast Bond Slow Bond Mega Bond XP BOND™

NEW!
Universal Total-Etch Adhesive
* For indirect indications in combination with DENTSPLY Self Cure Activator.

There are many adhesives available. Some bond a little better, others are
easy to use and again others are more forgiving. The new total-etch adhesive
XP BOND™ unites all these attributes in one single product.

XP BOND™ stands out because it delivers superior bonding performance

combined with easy handling and a high degree of technique tolerance.
Moreover, it is truly universal for all kinds of direct and indirect indications.*

Who needs the rest, when you can have it all inclusive?

Satellite Symposium on Dental Adhesives,
Dublin, September 13th, 2006
Dear ColIeagues,
I clearly remember the moment: During a German conserv-
ative dentistry congress focusing on adhesive vs conven-
tional techniques in 2004, one of my colleagues said: “I do
not think that ‘adhesive dentistry’ really exists. Okay, there
is even a journal named like that. I admit that there may be
something like an adhesive technique in dentistry, but I don’t
think this is really a discipline.”
Now, two years later with the previously mentioned jour-
nal having received an impact factor of more than 2.2, the
world can see how important this discipline has become in
the dental literature.
For decades, Dentsply has been one of the leading com-
panies dealing with adhesion. This supplement is the sci-
entific result of a satellite symposium held in Dublin on Sep-
tember 13th, 2006, prior to the annual IADR/CED/PEF
meeting just around the corner from famous Trinity College.
Experts from all over the world (USA, Germany, Belgium,
Spain, Italy) met to exchange experiences with established
adhesive materials and the most recent Dentsply develop-
Vol 9, Supplement 2, 2007
Guest Editorial
ment, XP-Bond. We learned that Dentsply’s Sevriton actual-
ly was the first adhesive approach, dated years before
Buonocore’s fundamental publication. We heard that fa-
tigue measurement is one major tool in preclinical testing
and that differences in performance during in vitro testing
blur between etch-and-rinse and self-etching adhesives; it is
becoming more important to look at the individual product.
However, clinical trials are still the ultimate instrument to in-
vestigate dental biomaterials, such as bonded resin com-
posites or ceramic inlays.
It is an honor for me to welcome you to this supplement
of the Journal of Adhesive Dentistry, 2007. Enjoy reading!
Sincerely,
Roland Frankenberger
223
Sarrett

260 The Journal of Adhesive Dentistry

 THE JOURNAL OF

ADHESIVE
DENTISTRY
Contents Volume 9 • Supplement 2, 2007

223 Satellite Symposium on Dental Adhesives, Dublin, September 13th, 2006

Editorial Roland Frankenberger

227 Dental Adhesives …. How it All Started and Later Evolved

Reviews Karl-Johan M. Söderholm

231 Effectiveness of All-in-one Adhesive Systems Tested by Thermocycling Following

Short and Long-term Water Storage
Uwe Blunck/Paul Zaslansky

241 Clinical Bonding of a Single-step Self-etching Adhesive in Noncarious Cervical

Lesions
Jan WV van Dijken/Karin Sunnegårdh-Grönberg/Ebba Sörensson

245 Shear Bond Strength and Physicochemical Interactions of XP BOND

Mark A. Latta

249 Microshear Fatigue Testing of Tooth/Adhesive Interfaces

Marc Braem

255 Microleakage of Class V Composite Restorations Placed with Etch-and-Rinse

and Self-etching Adhesives Before and After Thermocycling
Juan Ignacio Rosales-Leal

261 Microleakage of XP BOND in Class II Cavities After Artificial Aging

Jürgen Manhart/Cordula Trumm

265 Six-month Clinical Evaluation of XP BOND in Noncarious Cervical Lesions

Uwe Blunck/Katharina Knitter/Klaus-Roland Jahn

269 Adhesive Luting Revisited: Influence of Adhesive, Temporary Cement, Cavity

Cleaning, and Curing Mode on Internal Dentin Bond Strength
Roland Frankenberger/Ulrich Lohbauer/Michael Taschner/Anselm Petschelt/
Sergej A. Nikolaenko

275 XP BOND in Self-curing Mode used for Luting Porcelain Restorations.

Part A: Microtensile Test
Ornella Raffaelli/Maria Crysanti Cagidiaco/Cecilia Goracci/Marco Ferrari

279 XP BOND in Self-curing mode used for Luting Porcelain Restorations.

Part B: Placement and 6-month Report
Marco Ferrari/Ornella Raffaelli/Maria Crysanti Cagidiaco/Simone Grandini

Vol 9, Supplement 2, 2007 225

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Dental Adhesives …. How it All Started and Later Evolved
Karl-Johan M. Söderholma

Abstract: This article describes how dental adhesives evolved from the cements developed by the Mayan Indians into
today’s modern dental adhesives. Particular attention is paid to Oskar Hagger, a chemist who worked for DeTrey/Amal-
gamated Dental Company, and already in 1949 developed an adhesive product called Sevriton Cavity Seal. That adhe-
sive was acidic and interacted with the tooth surface on a molecular level. His ground-breaking concept makes him the
true “Father of Modern Dental Adhesives.” Hagger’s concept was soon adopted by other investigators, and different gen-
erations of dental adhesives evolved thereafter. Today, after many years of accepting that the key to the success of den-
tal adhesives is the micromechanical retention resulting from acid etching of dentin and enamel, we still return to Dr.
Hagger’s original concept that bonding can be achieved via molecular interactions between adhesives and tooth sur-
faces. That concept is obvious in the development of newer generations of dentin adhesives. These adhesives, like Sevri-
ton Cavity Seal, rely on acidic monomers capable of etching and interacting on a molecular level with tooth surfaces in
order to form physical/chemical bonds between the restoration and the tooth. Whether Hagger’s concept will become
the norm in the future is still an open question, but one thing is certain: Hagger’s idea is still very much alive.

Keywords: review, generations, clinical evaluations.

J Adhes Dent 2007; 9: 227-230. Submitted for publication: 15.12.06; accepted for publication: 4.1.07.

I n 1955, Buonocore published a paper entitled “A simple

method of increasing the adhesion of acrylic filling materi-
als to enamel surfaces”.15 That paper is often regarded as
the foundation of adhesive dentistry, and today that paper
is the 17th most cited paper published in the Journal of Den-
tal Research since March of 1919.
Buonocore’s paper15 clearly outlined different approach-
es to obtain bonding between filling materials and tooth
structure. These approaches included: (a) the development
of new materials which have adhesive properties, (b) modi-
fication of present materials to make them adhesive, (c) the
use of coatings as adhesive interface materials between fill-
ing and tooth, and (d) the alteration of the tooth surface by
chemical treatment to produce a new surface to which pre-
sent materials might adhere.
In the 1955 paper, Buonocore focused on the (d) alter-
native by targeting enamel bonding. He believed that treat-
a Professor, Department of Dental Biomaterials, College of Dentistry, University
of Florida, Gainesville, FL, USA.
Paper presented at Satellite Symposium on Dental Adhesives, Dublin,
September 13th, 2006.
Reprint requests: Prof. Karl-Johan M. Söderholm, Department of Dental Bioma-
terials, College of Dentistry, College of Dentistry, 1600 SW Archer Road,
Gainesville, FL 32610-0446, USA. Tel: +1-352-392-0575, Fax: +1-352-392-7808.
e-mail: ksoderholm@dental.ufl.edu
ment of intact enamel surfaces would have only limited ap-
plication to the broader problems of restorative dentistry. He
focused on enamel etching because he had found that phos-
phoric acid or preparations containing phosphoric acid had
been used to treat metal surfaces in order to obtain better
adhesion of paint and different resin coatings.
Obviously, Buonocore used knowledge from other disci-
plines and transferred that knowledge to dentistry. What
Buonocore did not seem to consider was that the Mayan In-
dians in pre-Columbian times had used acidic cements to at-
tach their semi-precious stone inlays.20 He also forgot to
consider that several acidic cements had been used by den-
tists more than a hundred years before he invented acid
etching,27 and that a common zinc phosphate cement was
a mixture of zinc oxide and phosphoric acid.37 It was well
known that during setting, these cements remained
acidic.40 What Buonocore forgot was that these cements
were also able to etch tooth surfaces and increase the sur-
face roughness. During setting, formed setting compounds
grew into the surface roughnesses created by the acidic ce-
ment. Because of mechanical interlocking between tooth,
cement, and crown, retention of the cemented restoration
could be achieved. Considering that the Maya were the first
to use acidic cements, a legitimate question is whether
Buonocore really was the one who invented acid etching or
if that honor shouldn’t go to the Maya. Buonocore’s true con-
tribution was that he opened our eyes to make us aware of

Vol 9, Supplement 2, 2007 227

Söderholm
Fig 1 Sevriton and Severiton Cavity seal were products devel-
oped by the DeTrey/Amalgamated Dental Company. Sevriton Cav-
ity Seal was the first product claimed to be able to bond to tooth
tissues.29 This product was developed by the Swiss chemist,
Oskar Hagger.
the fact that microscopic porosities enhanced the retention
of dental materials. What he did not communicate clearly,
though, was that by replacing a brittle cement layer with a
ductile material, the bonding ability could be substantially
enhanced. The latter fact was probably the reason why the
acid etching technique resulted in a major breakthrough in
dentistry when compared to previous approaches to bond-
ing to teeth.
However, when it comes to a ductile interface, Buonocore
was not the first to use a ductile resin layer at the tooth sur-
face in order to enhance retention. The first one who came
up with that idea was a Swiss chemist, Oskar Hagger. Hag-
ger worked for DeTrey/Amalgamated Dental Company, and
had already in 1949 developed an adhesive product called
Sevriton Cavity Seal33 (Fig 1). This product consisted of glyc-
erolphosphoric acid dimethacrylate and was intended for
use as an adhesive for the chemically cured resin Sevriton.
Sevriton Cavity Seal was indeed a revolutionary product, be-
cause it was the first product that claimed to be able to
chemically bond to tooth structure. In an article published by
Kramer and McLean in 1952,29 these two investigators
claimed that the glycerolphosphoric acid dimethacrylate of
the Sevriton Cavity Seal increased the adhesion to dentin by
penetrating the surface. Today we call the resin-penetrated
zone the hybrid zone. This is also remarkable, because we
often assume that hybridization is a more recent discovery
than it obviously is.
The year after Buonocore published his classic paper, he
also published a paper with Brudevold and Wileman,13 in
which they evaluated Sevriton Cavity Seal and Sevriton. In
that paper they claimed that the glycerolphosphoric acid
dimethacrylate did not bond as well to enamel as a self-cur-
ing resin placed in intimate contact with a phosphoric-
acid–etched enamel surface did. However, when placed in
228
contact with dentin, the glycerolphosphoric acid dimethacry-
late provided some dentin bond enhancement.
Considering Hagger’s fundamental work, there is no
doubt that modern dental adhesive technology had its root
in the late 1940s, when Hagger initiated the use of acidic
monomers to achieve bonding to both enamel and dentin.
What Buonocore really showed was that it was easier to
achieve bonding to enamel than to dentin, something we all
agree upon today.
Even though Buonocore had proved that enamel bonding
worked in 1955,15 it would take until the late 1970s before
enamel bonding became generally accepted. The turning
point occurred when 3M sponsored the International Sym-
posium on Enamel Etching in December of 1974.38 During
that symposium, researchers and clinicians with experience
of enamel bonding presented their findings, and 3M pub-
lished and distributed that information to academic institu-
tions and opinion leaders.
The idea to develop a resin system capable of bonding to
dentin did not die with Hagger. Instead, Bowen, after his in-
vention of modern composites, focused on dentin adhesives
during the 1960s. During that decade, he formed work
groups that outlined strategies for developing new dental ad-
hesives.7-11 Guiding principles during these discussions
were: (a) dentin is a vital tissue and should not be exposed
to strong acids, (b) the presence of water should be mini-
mized, because water would shield bond sites of adhesive
molecules, (c) the adhesive molecules should be at least bi-
functional so one end could bond to tooth surface and the
other to the resin of the composite.
As a result of Bowen’s research, NPG-GMA (N-phenyl-
glycine and glycidyl methacrylate) was introduced in 1965 as
a potential dentin adhesive. The shear bond strength of this
first generation adhesive was 1 to 3 MPa, and it soon be-
came obvious that these products did not work clinically.
During the late 1970s, new dentin adhesives were devel-
oped. Most of these products contained of bis-GMA/HEMA
resins mixed with halophosphorous esters. The bonding
mechanism of these adhesives was believed to be due to
ionic bond formation between halophosphorous groups and
calcium ions of the tooth surface. Even though these second
generation products were significant improvements com-
pared to the first generation products, they still did not result
in clinical success.
A major breakthrough occurred in 1979, when Fusayama
and his coworkers presented their findings, claiming they
could bond to acid-etched dentin without any significant
problems with pulp reactions.22 The paper was met with am-
ple skepticism by authorities in pulp biology who argued
that the acidity would cause pulp inflammations and even
pulp necrosis. Fusayama, on the other hand, argued that his
findings were just supporting Brännström and Nyborg’s
claim that bacteria rather than acid was the key concern
when it came to causing pulp damage.12
Another important paper from Japan came in 1982,
when Nakabayashi and coworkers published their paper
“The promotion of adhesion by the infiltration of monomers
into tooth substrates”. This paper presented the hybrid-lay-
er formation theory.35
The findings from Fusayama’s and Nakabayashi’s groups
The Journal of Adhesive Dentistry

resulted in a new generation of adhesives, the so-called 3rd
generation adhesives. Manufacturers of adhesives were still
somewhat reluctant to suggest an aggressive acid etching of
the dentin. Instead, they tried to remove or modify the smear
layer with a conditioner (often a weaker acidic solution) that
was rinsed away before a hydrophilic primer was placed.
These primers often consisted of 4-META and BPDM, and af-
ter primer application, an unfilled resin was placed. Other
primers contained PENTA, HEMA and ethanol. One product
used EDTA instead of acid to remove the smear layer and ex-
pose the collagen, and treated the exposed collagen fibers
first with an aldehyde and then HEMA.34 With that treat-
ment, it was believed that the aldehyde would chemically
bond to the collagen fiber and that the HEMA would then
bond to the attached aldehyde molecules via a condensa-
tion reaction. The methacrylate groups of the HEMA mole-
cule would then react with the composite.
Interesting to mention is that Bowen and Cobb published
a paper in 1983 entitled “A method for bonding to dentin
and enamel”,6 in which they claimed they could achieve an
in vitro tensile bond strength corresponding to one ton per
square inch. Translated into metric units, that would be 15.5
MPa. The bonding procedure was rather complex, but in that
article, Bowen regarded this approach as a major break-
through despite its complexity.
Even though the 3rd generation adhesives were im-
provements, they did not result in long-term success. In
1985, Hansen and Asmussen correlated gap sizes around
standardized cavities with the shear bond strength and
found that gap-free restorations would be possible at shear
bond strength values of around 23 MPa.25 The best adhe-
sives then had shear strength values of 18 MPa.
Toward the end of the 1980s, some interesting research
was published. The first paper came in 1985, when Bowen
presented an abstract at an IADR meeting that contained in-
formation on the NTG-GMA he had been so enthusiastic
about in his and Cobb’s 1983 publication.5 In the 1985 pre-
sentation, he revealed that the adhesive he had used in
1983 contained an impurity. That impurity was nitric acid,
and after purifying, the bond strength declined substantial-
ly. What he inadvertantly showed was how important it was
to etch the dentin surface.
Another important finding came in 1989, when Chigira et
al treated an EDTA-conditioned dentin surface with alde-
hyde plus HEMA or HEMA only and found no difference in
bond strength.17 What they showed with that study was that
collagen exposure and resin infiltration was the key behind
dentin bonding, thereby supporting Nakabayashi’s hy-
bridization theory.
Some of the most important information came in 1994,
when Van Herle’s group at the Catholic University of Leuven
showed in a clinical study that the success rate of Scotchbond
2, a third generation dentin adhesive, exceeded 95% after 3
years.43 Because of poor storage stability, Scotchbond 2 dis-
appeared from the market almost immediately after it had
been accepted and was replaced by Scotchbond MP, a 4th
generation adhesive. At that time, it had started to become
clear that by using more aggressive dentin treatments, the
bond strength improved and exceeded the levels predicted by
Hanssen and Asmusen for gap-free restorations.25
Vol 9, Supplement 2, 2007
Söderholm
Even though Fusayama and later on Nakabayashi had
done extensive research on dentin etching and dentin bond-
ing during the 1980s, it was during the early 1990s that
dentin etching and dentin bonding first became widely ac-
cepted. The acceptance coincided with a symposium spon-
sored by 3M and later on published in Operative Dentistry.4
Another important discovery was when Kanka28 and Gwin-
nett24 in two independent papers showed that bonding to
dentin could be enhanced by using so-called moist bonding.
Knowledge transfer is rarely an easy task, and when it
came to introducing the 4th generation adhesives to the
dental profession, it was soon clear that dentists did not re-
ally know how to do dentin bonding. Sometimes different
components were used in the wrong order, and when it came
to moist dentin, the definition differed quite widely. Because
of these factors, there was a need for products that were
easier to use, a demand to which the manufacturers soon
responded.
In an attempt to simplify dentin bonding, the primer and
adhesive resin were combined. Unfortunately, the general
perception among clinicians was often that by using a 5th
rather than a 4th generation adhesive, the time needed for
the bonding procedure could be decreased. In reality,
though, such a belief was incorrect, because these systems
required more time for the primer to diffuse into the collagen
structure. Clinical studies that came out comparing the 4th
and the 5th generation adhesives often suggested that the
4th generation adhesives performed somewhat better than
the 5th generation adhesives.1,14,31,42 Whether that differ-
ence was due to 5th generation adhesives curing too quick-
ly has not been proven. However, in vitro results of different
generation adhesives can be similar, independent of gener-
ation.19
Simultaneously with the introduction of the 5th genera-
tion adhesives, new adhesives consisting of an acidic primer
and an adhesive were also introduced. These systems often
came from Japanese manufacturers of dental adhesives,
and did not include the etching gel. Because of the genera-
tion terminology, these systems are referred to as the 6th
generation of adhesives.
In 1998, a new adhesive named Prompt-L-Pop was intro-
duced, consisting of a delivery system that mixed the primer
and the adhesive before it was applied. The popularity of this
system grew quickly and it soon became quite clear that the
market wanted a system that was self-etching and available
in one single container. During the past few years, the trend
has been to move the adhesive one step further by combin-
ing the acidic primer with the adhesive resin in an attempt
to develop an all-in-one system, often marketed as 7th gen-
eration adhesives.
The interest in the 7th generation products has been
quite significant, despite the fact that these systems often
perform less satisfactorily than many of the previous gener-
ation adhesives.39 However, it is important to emphasize
that all products, including the 7th generation adhesives,
have learning curves. The knowledge generated during
these trial periods is used to develop and improve products
that do not perform as well as originally believed. Unfortu-
nately, these development periods can be quite frustrating
for the clinicians when faced with patients who have re-
229
Söderholm
ceived a restoration that later fails. Today, most research in-
dicates that the 4th generation adhesives still serve as the
gold standard, but because of the interest dentists show in
the 7th generation adhesives, it seems clear that dentists
want simple-to-use adhesives. Because of that wish, they are
willing to explore adhesives that are easier to use, despite
the risk that they may have more failures with such products.
Thanks to what has been learned during that cycle of the
evolution process, these easier-to-use products have
evolved during the past few years, and today it seems that
the clinical success rate of 7th generation adhesives is ap-
proaching that of the 4th generation adhesives.2,3,16,18,21,23,
26,30,32,36,41,44
By looking back at adhesives, we must admit that
progress has been made since Hagger’s idea that resins
could be bonded to tooth surfaces. Nevertheless, we should
also remember that in 1949, when Hagger came up with his
revolutionary idea to use glycerolphosphoric acid dimetha-
crylate in Sevriton Cavity Seal, he had in fact invented a self-
etching adhesive. Based on the definitions, we can classify
Sevriton Cavity Seal as a 7th generation adhesive. Perhaps
improvements of dental materials don’t occur as fast as
many of us believe.
REFERENCES
1. Alhadainy HA, Abdalla AI. 2-year clinical evaluation of dentin bonding sys-
tems. Am J Dent 1996;9:77-79.
2. Aw TC, Lepe X, Johnson GH, Mancl L. One-year clinical evaluation of an
ethanol-based and a solvent-free dentin adhesive. Am J Dent 2004;17:451-
456.
3. Aw TC, Lepe X, Johnson GH, Mancl LA. A three-year clinical evaluation of two-
bottle versus one-bottle dentin adhesives. J Am Dent Assoc 2005;136:311-
322.
4. Barkmeier WW. International Symposium on adhesives in dentistry. Oper
Dent 1992;Suppl 5.
5. Bowen RL, Blosser RL, Johnston AD. Effects of ferric oxalate purity on adhe-
sive bonding to dentin [abstract 915]. J Dent Res 1985;64:276.
6. Bowen RL, Cobb EN. A method for bonding to dentin and enamel. J Am Dent
Assoc 1983;107:734-736.
7. Bowen RL. Adhesive bonding of various materials to hard tooth tissues. I.
method of determining bond strength. J Dent Res 1965;44:690-695.
8. Bowen RL. Adhesive bonding of various materials to hard tooth tissues. II.
Bonding to dentin promoted by a surface-active comonomer. J Dent Res
1965;44:895-902.
9. Bowen RL. Adhesive bonding of various materials to hard tooth tissues.III.
Bonding to dentin improved by pre-treatment and the use of surface-active
comonomer. J Dent Res 1965;44:903-905.
10. Bowen RL. Adhesive bonding of various materials to hard tooth tissues. IV.
Bonding to dentin, enamel, and fluorapatite improved by the use of a surface-
active comonomer. J Dent Res 1965;44:906-911.
11. Bowen RL. Adhesive bonding of various materials to hard tooth tissues. VI.
Forces developing in direct-filling materials during hardening. J Am Dent As-
soc 1967;74:439-445.
12. Brännström M, Nyborg H. The presence of bacteria in cavities filled with sili-
cate cement and composite resin materials. Sven Tandlak Tidskr
1971;64:149-155.
13. Brudevold F, Buonocore M, Wileman W. A report on a resin composition ca-
pable of bonding to human dentin surfaces. J Dent Res 1956;35:846-851.
14. Brunton PA, Cowan AJ, Wilson MA, Wilson NH. A three-year evaluation of
restorations placed with a smear-layer-mediated dentin bonding agent in
non-carious cervical lesions. J Adhes Dent 1999;1:333-341.
15. Buonocore M. A simple method of increasing the adhesion of acrylic filling
materials to enamel surfaces. J Dent Res 1955;34:849-853.
16. Burrow MF, Tyas MJ. Two-year clinical evaluation of One-Up Bond F in non-
carious cervical lesions. J Adhes Dent 2005;7:65-68.
230
17. Chigira H, Manabe A, Itoh K, Wakumoto S, Hayakawa T. Efficacy of glyceryl
methacrylate as a dentin primer. Dent Mater J 1989;8:194-199.
18. Dalton Bittencourt D, Ezecelevski IG, Reis A, Van Dijken JW, Loguercio AD. An
18-months' evaluation of self-etch and etch & rinse adhesive in non-carious
cervical lesions. Oper Dent 2005;30:275-281.
19. Dunn WJ, Söderholm KJ. Comparison of shear and flexural bond strength
tests versus failure modes of dentin bonding systems. Am J Dent 2001;
14:297-303.
20. Fastlicht S. Tooth Mutilations and Dentistry in Pre-Columbian Mexico. Chica-
go: Quintessence 1976.
21. Federlin M, Thonemann B, Schmalz G, Urlinger T. Clinical evaluation of dif-
ferent adhesive systems for restoring teeth with erosion lesions. Clin Oral In-
vestig 1998;2:58-66.
22. Fusayama T, Nakamura M, Kurosaki N, Iwaku M. Non-pressure adhesion of
a new adhesive restorative resin. J Dent Res 1979;58:1364-1370.
23. Gallo JR, Burgess JO, Ripps AH, Walker RS, Ireland EJ, Mercante DE, David-
son JM. Three-year clinical evaluation of a compomer and a resin composite
as Class V filling materials. Oper Dent 2005;30:275-281.
24. Gwinnett AJ. Moist versus dry dentin: its effect on shear bond strength. Am
J Dent 1992;5:127-129.
25. Hansen EK, Asmussen E. A comparative study of dentin adhesives. Scand J
Dent Res 1985;93:280-287.
26. Helbig EB, Klimm HW, Schreger IE, Haufe E, Natusch I. Controlled clinical
study of the anterior composite-adhesive system Point 4/OptiBond Solo Plus.
Schweiz Monatsschr Zahnmed 2002;112:1230-1235.
27. Hoffmann-Axthelm W. History of Dentistry. Chicago: Quintessence, 1976:
293-295.
28. Kanca J 3rd: Resin bonding to wet substrate. 1. Bonding to dentin. Quintes-
sence Int 1992; 23:39-41.
29. Kramer IRH, McLean JW. The response of the human pulp to self-polymeris-
ing acrylic. Br Dent J 1952;93:150-153.
30. Kubo S, Kawasaki K, Yokota H, Hayashi Y. Five-year clinical evaluation of two
adhesive systems in non-carious cervical lesions. J Dent 2006;34:97-105.
31. Mandras RS, Thurmond JW, Latta MA, Matranga LF, Kildee JM, Barkmeier
WW. Three-year clinical evaluation of the Clearfil Liner Bond system. Oper
Dent 1997;22:266-270.
32. Matis BA, Cochran MJ, Carlson TJ, Guba C, Eckert GJ. A three-year clinical
evaluation of two dentin bonding agents. J Am Dent Assoc 2004;135:451-
457.
33. McLean JW. Historical Overview: The pioneers of Enamel and dentin bond-
ing. In: Roulet J-F, Degrange M (eds). Adhesion – The silent revolution in den-
tistry. Chicago: Quintessence, 2000;13-17.
34. Munksgaard EC, Assmussen E. Bond strength between dentin and restora-
tive resins mediated by a mixture of HEMA and glutaraldehyde. J Dent Res
1984;63:1087-1089.
35. Nakabayashi N, Kojima K, Masuhara E. The promotion of adhesion by the in-
filtration of monomers into tooth substrates. J Biomed Mater Res 1982 ;
16:265-273.
36. Perdigao J, Carmo AR, Geraldeli S. Eighteen-month clinical evaluation of two
dentin adhesives applied on dry vs moist dentin. J Adhes Dent 2005;7:253-
258.
37. Servais Ge, Cartz L. Structure of zinc phosphate dental cement. J Dent Res
1971;50:613-620.
38. Silverstone LE, Dogon II. Proceedings of an international symposium on. The
Acid Etch Technique. St. Paul: North Central, 1975.
39. Söderholm KJ, Guelmann M, Bimstein E. Shear bond strength of one 4th and
two 7th generation bonding agents when used by operators with different
bonding experience. J Adhes Dent 2005;7:57-64.
40. Stanley HR, Going RE, Chauncey HH. Human pulp response to acid pretreat-
ment of dentin and to composite restoration. J Am Dent Assoc 1975;91:817-
825.
41. Türkün SL. Clinical evaluation of a self-etching and a one-bottle adhesive sys-
tem at two years. J Dent 2003;31:527-534.
42. van Dijken JW. Clinical evaluation of three adhesive systems in class V non-
carious lesions. Dent Mater 2000;16:285-291.
43. Van Meerbeek B, Braem M, Lambrechts P, Vanherle G. Evaluation of two
dentin adhesives in cervical lesions. J Prosthet Dent 1994;72:672-673.
44. Van Meerbeek B, Kanumilli PV, De Munck J, Van Landuyt K, Lambrechts P,
Peumans M. A randomized, controlled trial evaluating the three-year clinical
effectiveness of two etch & rinse adhesives in cervical lesions. Oper Dent
2004;29:376-385.
The Journal of Adhesive Dentistry
Effectiveness of All-in-one Adhesive Systems Tested by
Thermocycling Following Short and Long-term Water
Storage
Uwe Bluncka/Paul Zaslanskyb

Purpose: To evaluate and compare the marginal integrity of in vitro Class V restorations made with all-in-one adhesive
systems by thermocycling after different periods of water storage, to provide an analysis of static and quasi-dynamic
deterioration in water.

Materials and Methods: Standardized Class V cavities (17 groups, 8 specimens each) were prepared in extracted
human caries-free anterior teeth. The cavities were filled using 14 all-in-one adhesive systems/composite resin com-
binations in addition to the multi-bottle adhesive systems Syntac and OptiBond FL (etch-and-rinse technique) and
Clearfil SE Bond (self-etching) as controls. The samples were thermocycled after water storage for 21 days, after 1
year and again after 3 years (2000 cycles between 5 and 55°C) and replicas were made before and after each ther-
mocycling treatment (TC) for quantitative marginal analysis in the SEM.

Results: In dentin, marginal adaptation showed no significant differences between all groups after the first TC. After
one year of water storage and a second TC, the results for Prompt L-Pop (1999), Adper Prompt L-Pop/Tetric Ceram,
and One-up Bond F Plus showed a statistically significant decrease of margin quality 1 (MQ1) score compared to the
reference groups. When the all-in-one adhesives G-Bond, AQ-Bond, Hybrid Bond, and One-up Bond F Plus were used,
the enamel margins of restorations showed lower percentages of “continuous margins” (p < 0.05) after 1 year of
water storage and TC. Of the materials tested after 3 years of water storage and TC, only AQ Bond had a significantly
lower MQ1 score.

Conclusion: While all materials exhibited deterioration in the MQ1 quality score, the rate of deterioration varied, and
the results show that different materials have different deterioration rates after initial vs long-term water storage. The
deterioration along margins in dentin was not as extensive as predicted from other studies; however, the results from
the enamel margins show that one-bottle all-in-one adhesives seem to be significantly affected by water storage. The
results of this study suggest that the all-in-one adhesive group members perform very differently from each other:
thus, data need to be explored further at the level of each different adhesive product

Keywords: marginal quality evaluation, in vitro Class V restorations, adhesive system effectiveness.

J Adhes Dent 2007; 9: 231-240. Submitted for publication: 15.12.06; accepted for publication: 4.1.07.

A dhesive systems are routinely used to improve the mar-

a Associate Professor, Charité-Universitätsmedizin Berlin, Dental School, Campus
Virchow Klinikum, Berlin, Germany.
b Staff Scientist, Max Planck Institute of Colloids and Interfaces, Department of
Biomaterials, Potsdam, Germany
Paper presented at Satellite Symposium on Dental Adhesives, Dublin,
September 13th, 2006.
Reprint requests: Dr. Uwe Blunck, Charité-Universitätsmedizin Berlin, Dental
School, Campus Virchow Clinic, Augustenburger Platz 1, 13353 Berlin, Germany.
Tel: +49-30-450-562-673, Fax: +49-30-450-562-961.
ginal seal of composite resin restorations at the inter-
faces with enamel and dentin. Bonding between enamel or
dentin and the restorative composite must be sufficiently ef-
fective to resist the varying stresses to which a “typical”
restoration is subjected. Such stresses include the poly-
merization shrinkage during composite placement as well as
mechanical, thermal, and hydration stresses incurred in the
oral environment due to normal use and wear.25
Available adhesive systems may be classified as dentin-
conditioning adhesive systems with selective acid etching
on enamel, etch-and-rinse systems which necessitate phos-
phoric acid etching and rinsing of enamel/dentin prior to ap-

Vol 9, Supplement 2, 2007 231

Blunck/Zaslansky

Table 1 Tested adhesive system/composite resin combinations

Group Adhesive system Composite resin Adhesive manufacturer

Multi-bottle systems Syntac Artemis Ivoclar Vivadent; Schaan,

(control) Liechtenstein
OptiBond FL Herculite XR Kerr; Danbury, CT, USA
Clearfil SE Bond Clearfil AP-X Kuraray; Tokyo, Japan

All-in-one Prompt L-Pop 1999 Tetric Ceram ESPE; Seefeld, Germany

adhesive systems Prompt L-Pop 2000 Tetric Ceram ESPE
with mixing Adper Prompt L-Pop Tetric Ceram 3M ESPE; St Paul, MN, USA
Adper Prompt L-Pop Filtek Z250 3M ESPE
Futurabond NR Grandio Voco; Cuxhaven, Germany
One-up Bond F Estilite Tokuyama; Tokyo, Japan
Xeno III Tetric Ceram Dentsply DeTrey; Konstanz, Germany
Xeno III Dyract eXtra Dentsply DeTrey
Xeno III Quixfil Dentsply DeTrey

All-in-one AQ Bond Metafil CX Morita; Irvine, CA, USA

adhesive systems G-Bond Gradia GC; Tokyo, Japan
without mixing Hybrid Bond Metafil Morita
iBond Charisma Heraeus Kulzer, Hanau, Germany
tri-S bond Clearfil AP-X Kuraray

plying multi-bottle or one-bottle adhesives, and self-etching MATERIALS AND METHODS

systems that contain acid monomers which can condition
both enamel and dentin simultaneously with no rinsing.36
Self-etching adhesive systems can be applied in two con-
secutive steps or as so-called all-in-one adhesives. The lat-
ter are available in two forms: those that require mixing and
those that do not.
The effectiveness of adhesive systems can be tested in
vitro by bond strength measurements of various kinds, by
penetration tests of Class V/II fillings with different sub-
stances, and by evaluating the margin quality of Class I/II/V
or cylindrical fillings under a microscope.17 In this study, vi-
sual inspection of discontinuities at the margins was per-
formed using a scanning electron microscope (SEM), dedi-
cated to the identification and quantification of dental mar-
gin qualities.26 This method has several advantages, such
as the high level of detail revealed and marked accuracy, al-
lowing it to be used for evaluating the same margins at dif-
ferent times. This is particularly useful for testing the effects
of water storage or stress on the same specimens.
This paper considers the effectiveness of all-in-one ad-
hesive systems in comparison to reference multi-bottle ad-
hesive systems, as judged by evaluating the marginal in-
tegrity in dentin and enamel after different periods of water
storage. The effects of short- vs long-term storage were ex-
emplified by applying thermal stress in order to expose mar-
ginal degradation differences. This was used to study the
state of the restoration margins at 3 weeks, 1 year and 3
years, and consider some aspects of the dynamics of adhe-
sive aging.
This work reflects the current status of a large ongoing study.
Teeth, anonymously collected following routine dental treat-
ment, were stored in 0.1% thymol solution at room temper-
ature prior to and during the experimental period. One hun-
dred thirty-six caries-free extracted human anterior teeth
were used, and typical Class V cavities were prepared with
a diamond bur (diamond bur No. 838/314/014; Gebr. Bras-
seler; Lemgo, Germany) at high speed using water as a
coolant. Oval preparations were a standard size: approxi-
mately 4 mm high, 1.5 mm deep, and 3 mm wide (2 mm api-
cal to the cementoenamel junction spanning across the CEJ
and into enamel). The enamel portions were bevelled with a
finishing diamond bur (Composhape H-15, Intensiv; Vi-
ganello-Lugano, Switzerland) and the cavosurface margins
in dentin finished to a 90-degree angle with a finishing dia-
mond (No. 8838/314/012, Gebr. Brasseler). The teeth were
randomly divided into 17 groups of 8 teeth each.
Each group of teeth was assigned to one of 17 treat-
ments. These included 14 combinations of all-in-one adhe-
sive system/composite resins and three multi-bottle adhe-
sive systems (Syntac and OptiBond FL, etch-and-rinse tech-
nique, and Clearfil SE Bond, self-etching technique). The ad-
hesives were all applied and restored with composite resin
according to the manufacturer’s instructions as detailed in
Table 1. In an attempt to ensure optimal performance of the
adhesives, the composite used was generally that recom-
mended by the adhesive manufacturer, although for some
of the adhesives (Adper Prompt L-Pop and Xeno III), several

232 The Journal of Adhesive Dentistry


composites were used. The composite resin was inserted in
two increments (initially placed at the cervical margin), and
each increment was light cured (Astralis 10 light-curing unit,
Ivoclar Vivadent; Ellwangen, Germany) for 40 s. After finish-
ing and polishing (Sof-Lex Pop-on Nr. 1981 SF/F/M/C 3M
ESPE; St Paul, MN, USA), the teeth were returned to water
storage for 21 days, followed by 2000 cycles of thermocy-
cling (TC) between +5 and +55°C.
Prior to and after TC, impressions were taken with a
polyvinylsiloxane material (Silagum light body, DMG; Ham-
burg, Germany) and replicas of the restoration and sur-
rounding tooth structures were produced. These were cast
with an epoxy resin following precise manufacturer guide-
lines (Stycast 1266 Part A + B; Emerson and Cumming; West-
erlo-Oevel, Belgium). Once fully cured, each replica was sput-
ter-gold coated (SCD 030, Balzers Union; Balzers, Liechten-
stein) in preparation for inspection by SEM. Similar impres-
sion and TC procedures were repeated after 1 year of water
storage, and for 11 products also after 3 years.
The effectiveness of each bonding system was assessed
by evaluating the margins of the restorations at the
dentin/composite and enamel/composite interface. Mea-
surements were performed using a dedicated SEM (AMRAY
1810, Amray; Bedford, MA, USA) and all replicas were viewed
at a magnification of 200X, and classified according to the
state of the margin in different areas in order to numerical-
ly quantify the marginal qualities, as detailed in Table 2. By
using this method, each segment of the tooth/restoration in-
terface was imaged and ranked according to defined quali-
ty criteria. These were then converted into percentage of the
total margin length, in dentin and enamel independently.
Statistical evaluation was performed using an SPSS sta-
tistical software package (SPSS Software; München, Ger-
many). Within each sample group, significant differences
were determined using the nonparametric Wilcoxon test. For
comparison between the different treatment groups, the
nonparametric Kruskal-Wallis test was used followed by Bon-
ferroni adjustment. The statistics were calculated for the pa-
rameter margin quality 1 (MQ1 = “excellent” or “continuous”
margin). Origin 7.0 SR0 (Originlab; Northampton, MA, USA)
was used for the weighted regression and Microsoft Excel
(2000) was used to determine the slopes between MQ1
rankings at different stages of the experiment.
RESULTS
The results of the 14 test groups were compared with those
of the 3 reference multi-bottle adhesives OptiBond FL, Syn-
tac, and Clearfil SE Bond. Figure 1 is a box-and-whiskers plot
of the marginal quality MQ1results determined for the enam-
el margins, depicting the median, 25 and 75 percentiles.
The main result seen here is that after 1 year of water stor-
age (Fig 1a) and following a second TC, a reduction (signifi-
cant at p < 0.05) in the amounts of “continuous margins”
(MQ1) is seen for G-Bond, AQ-Bond, Hybrid Bond, and One-
up Bond F Plus. No significant difference was found between
any other of the groups and the reference adhesives. After
3 years of water storage and a third TC, only AQ Bond had a
substantially lower MQ1 score (p < 0.05).
Vol 9, Supplement 2, 2007
Blunck/Zaslansky
Table 2 Criteria for the marginal analysis in the SEM
Margin
quality Definition
1 Margin not or hardly visible, no or slight marginal
irregularities*; no gap
2 No gap but severe marginal irregularities*
3 Gap visible (hairline crack up to 2μm, no marginal
irregularities*
4 Severe gap (more than 2μm), slight and severe
marginal irregularities*
* The term "marginal irregularities" refers to porosities, marginal
restoration fracture, or bulge in the restoration
Figure 2 shows the MQ1 results that were obtained for
each product in dentin following each of the three TC treat-
ments. Following the first TC (Fig 2a), no statistically signifi-
cant differences were found for any of the groups. The TC af-
ter 1 year of water storage (Fig 2b) revealed a decrease in
MQ1 for Prompt L-Pop in the 1999 version, Adper Prompt L-
Pop/Tetric Ceram, and One-up Bond F Plus (p < 0.05). After
three years of water storage and a 3rd TC both Prompt L-Pop
(1999) and Adper Prompt L-Pop/Tetric Ceram were found to
have substantially lower MQ1 scores than the reference
groups (p < 0.05). Data for One-up Bond F Plus, G-Bond, AQ-
Bond, Hybrid Bond, and tri-S Bond are missing for three
years, as these materials were not available for the full du-
ration of the present study.
To better understand the dynamics of the results pre-
sented in Fig 2 and to obtain insights into the effects of TC
and water storage, plots were produced of MQ1 for each
group before and after TC at 21 days (T1 and T2), after 1 year
of water storage (T3 and T4) and after 3 years of water stor-
age (T5 and T6). Only the plots for the reference multi-bottle
products are shown as examples in Fig 3. Each data point
(T1-T6) represents the median MQ1 values with the corre-
sponding error bars that are the standard error of the mean
(SE). It must be emphasized that in these plots, the time in-
tervals between the data points are not equal. The trends of
the T1-T2, T2-T4, and T4-T6 segments were calculated in
each graph, because the effects of water storage alone (seg-
ment T2-T3 after 1 year and segment T4-T5 after 2 addi-
tional years) were too small to be directly and reliably visu-
alized. Thus, the purpose of TC was to challenge the bonds
of the restorations in order to test the marginal integrity. Fur-
ther analysis was then used to explore the joint effects of TC
after the different water storage periods.
The T1-T2, T2-T4, and T4-T6 slopes as well as the statisti-
cal significance (p) of the difference between each pair of the
corresponding MQ1 values (obtained with the nonparamet-
ric Wilcoxon rank test) are presented in Table 3, columns A to
F (shown as 1st water storage [WS] vs 1st TC, 1st TC vs 2nd TC,
2nd TC vs 3rd TC). We also calculated trends in the overall ad-
hesive effectiveness by fitting linear regression lines (error
233
Blunck/Zaslansky

0 20 40 60 80 100 %
+ Syntac
OptiBond FL
Clearfil SE Bond

Prompt L-Pop 1999

Prompt L-Pop 2000
+ Adper Prompt L-Pop / Tetric Ceram
MQ1 Adper Prompt L-Pop / Filtek Z250
results after Xeno III / Quixfil
a. 2 nd TC Xeno III / Tetric Ceram
enamel
Xeno III / Dyract eXtra
+ Futurabond NR
One-up Bond F Plus
*
* AQ
iBond
Bond

* G-Bond
* Hybrid Bond
tri-S bond

+ Syntac
OptiBond FL
Clearfil SE Bond

MQ1 Prompt L-Pop 1999

results after
b. 3 rd TC Prompt L-Pop 2000
enamel + Adper Prompt L-Pop / Tetric Ceram
Adper Prompt L-Pop / Filtek Z250
Xeno III / Tetric Ceram Fig 1 Results of marginal quality
Xeno III / Dyract eXtra 1 in % relative to the enamel mar-
gin length in Class V cavities for
* AQ Bond
iBond
self-etching adhesive systems
after (a) 1-year water storage and
a 2nd TC and (b) after after 3-
0 20 40 6 80 100 % year water storage and a 3rd TC
0 (o and + = outliers, * = statisti-
cally significantly different com-
pared to Syntac, Opti Bond FL,
and Clearfil SE Bond, p < 0.05).

weighted by the SE) through the six MQ1 data points for every
product. The slopes of these regression lines, as well as the
95% confidence intervals and r2 values are also shown in
Table 3 (columns I to L), and they provide an overall estimate
of the trend for the deterioration of the MQ1 results for each
product. A general linear deterioration was observed for all
groups (see example plots in Fig 3), which shows that the de-
terioration rate is not consistent over time. Furthermore, for
all the products, the overall trend (column I) only occasional-
ly corresponds to the trend of the intermediate segments
(columns A, C, E, and G in Table 3).
Finally, to better understand how well the data from the
first year can be used to predict the trend in the performance
of each product over a period of 3 years, the trends of T1 -
T4 were calculated and used to derive a percent deviation
estimate relative to the regressed overall trend (the differ-
ence divided by the slope of the overall trend as %, shown in
Table 3, column M). Note that for some of the products (Opti-
Bond FL, AQ Bond, Prompt L Pop 2000, Adper Prompt L Pop,
and Xeno III) a reasonable (≤ 10%) prediction was found,
while for others, deviations of 20%, 30% or even 40% exist.
DISCUSSION
Effectiveness of adhesive systems can be generally judged
by the marginal adaptation of composite resin restorations
at the interface with the tooth substrate. Marginal adapta-
tion is affected by many different parameters. These might
be greatly influenced by the inherent properties of the
restorative material, such as shrinkage and shrinkage
stress,24 the chemistry of the adhesive system used, the size

234 The Journal of Adhesive Dentistry

 Blunck/Zaslansky

0 20 40 60 80 100 %
Syntac
Optibond FL
Clearfil SE Bond
Prompt L-Pop (1999)
Prompt L-Pop (2000)
MQ1 Adper Prompt L-Pop / Tetric Ceram
a. results after
Adper Prompt L-Pop / Filtek Z250
1 st TC
dentin Xeno III / Dyract eXtra
Xeno III / Quixfil
+ Xeno III / Tetric Ceram
Futurabond NR
One Up Bond F Plus
AQ Bond
iBond
Hybrid Bond
G-Bond
tri-S bond
Syntac
OptiBond FL
Clearfil SE Bond

* Prompt L-Pop 1999

Prompt L-Pop 2000

* Adper Prompt L-Pop / Tetric Ceram

Adper Prompt L-Pop / Filtek Z250
MQ1 Xeno III / Dyract eXtra
results after Xeno III / Quixfil
b. 2 nd TC Xeno III / Tetric Ceram
dentin
Futurabond NR

* AQ Bond
One-up Bond F-Plus

iBond
Hybrid Bond
G-Bond
tri-S bond
Syntac
OptiBond FL
Clearfil SE Bond
Fig 2 Marginal quality 1 results MQ1
in % of the dentin margin length in c. results after
3 rd TC
* Prompt L-Pop 1999
Prompt L-Pop 2000
Class V cavities for all-in-one adhe-
sive systems after (a) 21 days of
dentin
+ * Adper Prompt L-Pop / Tetric Ceram
Adper Prompt L-Pop / Filtek Z250
water storage and a 1st TC, after Xeno III / Dyract eXtra
(b) 1 year of water storage and a + Xeno III / Tetric Ceram
2nd TC, and (c) after after 3 years
of water storage and a 3rd TC (o AQ Bond
and + = outliers, * = statistically iBond
significantly different compared to
0 20 40 6 80 100 %
Syntax, OptiBond FL, and Clearfil 0
SE Bond p < 0.05).

of the cavity, the c-factor,9 the insertion technique, and the
polymerization protocol.1
In this study, a high resolution quantitative marginal
analysis method was used to evaluate the marginal adapta-
tion of composite resin restorations over a long period of wa-
ter storage followed by TC. This quantification method relies
on imaging of precision replicas of restored teeth with a
scanning electron microscope, followed by quantitative qual-
ity analysis of the entire margin length. The replica technique
is non-destructive to the natural-tooth samples; hence, the
margins can be assessed and marginal defects detected
and compared at different times, as well as after applying
different stresses to the tooth specimens. The high sensi-
tivity of this method, due to the SEM's excellent detail re-
production, is a great advantage for the evaluation of such
bonding of adhesive systems.4,26
The results (Figs 1 and 2) show a distribution of the MQ1
results of the restoration margins at different stages of the

Vol 9, Supplement 2, 2007 235

Blunck/Zaslansky

[% MQ1]
100
95
90
a.
85 Optibond FL
80
75
T1 T2 T3 T4 T5 T6

[% MQ1]
100
95
90
b.
85 Syntac
80
75
T1 T2 T3 T4 T5 T6

[% MQ1]
100 Fig 3 Median MQ1 values in % of entire margin length
95 in dentin with error bars indicating the standard error of
90 the mean for the multi-bottle reference materials (a) Opti
c.
85 Clearfil SE Bond Bond FL, (b) Syntac and (c) Clearfil SE Bond at the six
evaluation stages T1 (after 21 days’ water storage), T2
80
(after 1st TC), T3 (after 1 year of water storage), T4 (after
75 2nd TC), T5 (after 3 years of water storage) and T6 (after
T1 T2 T3 T4 T5 T6 3rd TC). Black lines: regression lines weighted by the cor-
responding standard error; dotted lines: 95% confidence
intervals.

study, but overall the scores are quite high, perhaps due to
the fact that the deterioration is generally quite minimal.
Further examination of the present data allows creating a
quasi-dynamic perspective of the deterioration rate of the
restorations (Fig 3 and Table 3). Thus it is seen that there is
a general negative trend in the MQ1 values, when these are
determined after water storage and/or thermocycling (TC).
Clearly, the specific state of the bond between each
restorative and the tooth is not easily determined by any sur-
face-evaluation method, particularly following long-term wa-
ter storage. The decision was thus made to use TC to induce
mild stress to every tooth-restoration interface in order to bet-
ter reveal its state as determined by the marginal quality eval-
uation. As can be seen in Table 3, the effect of TC is not con-
stant during early vs late (> 1 year) water storage, and this is
attributed to the differences in the adhesive stability in wa-
ter. A number of publications have dealt with the effects of
similar long-term water storage beyond 2 years.2,3,7,16,22,
23,27 To the best of our knowledge, however, none have man-
aged to produce high-resolution long-term data mapping the
marginal quality deterioration on the same samples.
Despite the fact that the cavity dimensions were stan-
dardized, the amount of stress induced to the interface of
each restoration probably varied considerably. This might
be due to the large variations in the coefficients of thermal
expansion of each restorative28,29 or possibly due to tooth
variability. Be that as it may, because the manufacturer-rec-
ommended composites were used, it was assumed that the
conditions were optimal for each adhesive, and that the
best performance was obtained. It remains to be seen if oth-
er combinations of composite/adhesive deliver improved
long-term results. Possibly, a standard composite restora-
tive should be used for such tests in the future in order to
better compare the effectiveness of the investigated adhe-
sives. The importance of the effect of the composite resins
can clearly be seen in the groups of Adper Prompt L-Pop and
Xeno III, where large differences in MQ1 values and slopes
are seen for the same adhesive. Note however, that while
Adper Prompt L-Pop in combination with Tetric Ceram
showed a statistically significant decrease in MQ1 com-
pared to the results obtained with Filtek Z250, all three
combinations with Xeno III (Dyract XP, Quixfil, and Tetric Ce-
ram) revealed no statistically significant differences in mar-
ginal integrity. We therefore conclude that these adhesives
react differently to composite resins with higher polymer-
ization shrinkage stress values.
Both in vitro6,7,10,11 and in vivo studies8,12,13,35,37 have
shown that multi-bottle multi-step adhesive systems such as

236 The Journal of Adhesive Dentistry

 Table 3 Slopes of regression lines and statistical significance (p) of results from different evaluation stages after water storage (WS) and thermocycling (TC):
columns A + B = 1st WS vs 1st TC, columns C + D = 1st TC vs 2nd TC, columns E + F = 2nd TC vs 3rd TC, columns G + H = 1st WS vs 2nd TC. Columns I to L show the
slope for the regression lines for all data points of one group, r2-values, lower (LCI) and upper confidence intervals (UCI). The last column shows the percentage
of deviation between the slopes of the overall regression lines (column I) and the regression lines between 1st and 2nd TC (column C). n.a. = not analyzed (data
were not available after 3 years of water storage). Column M is the percent deviation calculated by the formula [100*(I col I - col G I/col I)] where col I and col
G refer to values in columns I and G, resp.

A B C D E F G H I J K L M
1st WS vs 1st TC 1st TC vs 2nd TC 2nd TC vs 3rd TC 1st WS vs 2nd TC r2 LCI UCI %

Vol 9, Supplement 2, 2007

slope p slope p slope p slope p Deviation

Syntac /
Artemis -2.36 0.173 -0.73 0.028 -0.53 0.028 -1.27 0.028 -0.97 0.91 -1.99 0.05 30.93
OptiBond FL /
Herculite XR -1.80 0.018 -1.26 0.069 -1.97 0.017 -1.44 0.017 -1.56 0.98 -2.65 -0.48 7.69
Clearfil SE Bond /
Clearfil AP-X 0.00 0.109 -4.33 0.018 -2.88 0.012 -1.53 0.018 -2.50 0.89 -3.41 -1.60 38.80
Prompt L-Pop 1999 /
Tetric Ceram -6.11 0.018 -21.99 0.012 -3.40 0.012 -16.70 0.012 -13.06 0.95 -15.45 -10.68 27.87
Prompt L-Pop 2000 /
Tetric Ceram -6.94 0.018 -4.01 0.093 -3.71 0.012 -4.99 0.012 -4.52 0.98 -5.80 -3.25 10.40
Adper Prompt L-Pop /
Tetric Ceram -6.23 0.018 -10.51 0.012 -6.17 0.012 -9.08 0.012 -8.55 0.98 -10.30 -6.81 6.20
Adper Prompt L-Pop /
Filtek Z250 -3.32 0.018 -3.69 0.012 -1.55 0.012 -3.56 0.012 -2.95 0.97 -3.83 -2.06 20.68
Xeno III /
Tetric Ceram -0.89 0.068 -2.13 0.043 -0.92 0.018 -1.72 0.028 -1.35 0.91 -2.78 0.07 27.41
Xeno III /
Dyract eXtra -2.61 0.043 -0.40 0.043 -0.84 0.012 -1.13 0.043 -1.09 0.92 -2.80 0.62 3.67
Xeno III /
Quixfil -1.77 0.138 -2.72 0.028 n.a. n.a. -2.40 0.028 -2.07 0.96 -4.65 0.51 15.94
Futurabond NR /
Grandio -3.83 0.028 -1.32 0.018 n.a. n.a. -2.15 0.018 -2.21 0.94 -4.34 -0.09 2.71
One-up Bond F Plus/
Estilite -6.43 0.012 -11.49 0.012 n.a. n.a. -9.80 0.012 -6.65 0.77 -12.77 -0.53 47.37
AQ Bond /
Metafil CX 0.00 0.109 -2.66 0.401 -1.60 0.069 -1.77 0.028 -1.63 0.96 -2.36 -0.90 8.59
Hybrid Bond /
Metafil -4.31 0.018 -1.83 0.018 n.a. n.a. -2.66 0.018 -2.62 0.95 -4.94 -0.30 1.53
iBond /
Charisma -0.95 0.043 -3.07 0.028 -0.95 0.012 -2.36 0.028 -1.83 0.95 -2.99 -0.68 28.96
G-Bond /
Gradia -4.22 0.012 -7.16 0.012 n.a. n.a. -6.18 0.012 -4.61 0.78 -8.44 -0.78 34.06
tri-S Bond /
Clearfil AP-X -6.20 0.012 -3.12 0.012 n.a. n.a. -4.15 0.012 -3.90 0.93 -6.03 -1.76 6.41

237
Blunck/Zaslansky
Blunck/Zaslansky

AQ Bond
21 days of WS v s. 1st TC
Clearfil SE Bond
Xeno III / Tetric Ceram
multi-bottle adhesiv es

all-in-one adhesiv es w ith mixing

* iBond
Xeno III / Quixfil

all-in-one adhesiv es w ithout mixing * OptiBond FL

a.
* Xeno III / Dyract eXtra
Syntac

* Adper Prompt L-Pop / Filtek Z250

* Futurabond NR
* G-Bond
*
* Hybrid Bond

* tri-S Bond
Prompt L-Pop 1999

* Adper Prompt L-Pop / Tetric Ceram

* One-up Bond F Plus
* Prompt L-Pop 2000
*
-25 -20 -15 -10 -5 0

1st TC v s. 2nd TC * Xeno III / Dyract eXtra

Syntac
OptiBond FL
multi-bottle adhesiv es

all-in-one adhesiv es w ith mixing

* Futurabond NR

* Xeno III / Tetric Ceram

Hybrid Bond

all-in-one adhesiv es w ithout mixing * AQ Bond

b.
* Xeno III / Quixfil

* tri-S Bond
iBond

*
* Adper Prompt L-Pop / Filtek Z250 Fig 4 Ranked slopes of regres-
Prompt L-Pop 2000 sion lines through MQ1 values
* Clearfil SE Bond in dentin for each product (a)
after 21 days of water storage
* Adper Prompt L-Pop / Tetric Ceram
G-Bond
vs 1st TC (column A in Table 3)
* One-up Bond F Plus and (b) 1st TC vs 2nd TC (col-
* Prompt L-Pop 1999 umn C in Table 3). * denotes
* stopes that were determined
between MQ1 median values
-25 -20 -15 -10 -5 0
that are statistically different
with p < 0.05 (Wilcoxon test).

OptiBond FL and Syntac in combination with the etch-and-
rinse technique and the multi-step self-etching adhesive
Clearfil SE Bond are reliable adhesives even after long-term
usage. For this reason, these three products were used as
reference materials in this study. They also provide to some
extent a means to calibrate the present results with other
studies. With the quasi-dynamic trends, it is possible to rank
the different adhesives according to their rate of deteriora-
tion (as shown for mainly after TC) after 21 days or 1 year in
water (see example Figs 4a and 4b). This ranking differs for
the two water storage periods, which can be attributed to the
specific properties of each adhesive, which lead to differ-
ences in bond quality and rates of degradation.
The working assumption of this study was that better per-
formance of any adhesive group would be associated with
the highest (least negative) slope of MQ1 deterioration (col-
umn I in Table 3). These slope values are different from the
slopes of the individual segments 1st WS vs 1st TC and 1st
vs 2nd TC, and thus the rate of deterioration of the bonds
might vary substantially over time. As seen in Figs 4a and 4b,

238 The Journal of Adhesive Dentistry


many of the products, change the rank between the initial
water storage period, as compared with the rank after the
first year . We are aware that such ranking might be of limit-
ed use for predicting clinical performance; therefore, clini-
cians and manufacturers might need to define criteria for
“adequate performance”, not “better performance”. Clearly
such long-term effects need to be considered in addition to
operation skill and experience,15,21 both of which are diffi-
cult to account for, therefore consequences of these findings
necessitate further investigations.
The marginal analysis centered on the quantitative eval-
uation of MQ1 (“excellent” or “continuous” margin) as a
measure for marginal integrity. It has recently been shown
that such an evaluation provides a good indicator for the
ability of an adhesive system to compensate for the shrink-
age of composite resins during polymerization, as compared
to bond strength tests.17 The extent to which the present in
vitro results correspond to in vivo data of quantitative mar-
ginal analysis of Class V fillings is not obvious, especially as
there are reports showing that such data are unable to pre-
dict clinical outcome.17 Nevertheless, results of this study
and trend analysis provide an additional means of deter-
mining objective and standard measures of the physical at-
tributes of any combination of adhesive system and com-
posites. It therefore remains to be seen just how such details
match the outcomes of clinical investigations. It is worth-
while to note that other studies have evaluated the margin-
al quality using stress induced by mechanical loading.12,13
The method employed in this study has the advantage that
TC induces precise and repeatable stress (assuming the co-
efficient of thermal expansion of the composites stays con-
stant), and this concept was used to provide more informa-
tion about the effects of water storage at short and long in-
tervals.
The present results are based on SEM evaluation of the
percentage of the different marginal qualities, calculated in
relation to the entire margin length in dentin or enamel in-
dependently. It has been shown that when the same opera-
tor evaluates the same specimens twice, the difference be-
tween the results is in the range of 4%,26 whereas when two
trained operators evaluate the same specimens, the differ-
ences can reach 10% to 20%.18 Therefore, all specimens in
this study were prepared and evaluated by the same opera-
tor.
It is interesting to note that for most of the products not
displaying a large discrepancy between the initial and inter-
mediate MQ1 values, the first-year data provide only a mod-
erate predictor for the longer term trend of deterioration.
Therefore, initial predictors of restorative success have lim-
ited applicability, and more data over long periods of time
are needed. This is unavoidable even in an in vivo setting,
and is important especially when both manufacturers and
clinicians want to know as early as possible which is the best
product. It is, of course, conceivable that storage at higher
temperatures might allow faster answers to these questions.
All-in-one adhesives are rather user friendly; however, cer-
tain indicators have suggested reduced performance that
might be associated with their usage. Compared with two-
step self-etching or etch-and-rinse adhesive systems, lower
bond strength values were reported.5,14,19,20 It has also
Vol 9, Supplement 1, 2007
Blunk/Zaslansky
been shown that permeable membranes develop after cur-
ing due to a high hydrophilicity, which allows water move-
ments through the all-in-one adhesive layer.30 Sites of in-
complete water removal and subsequent suboptimally poly-
merized resins31 have been described and termed “water
trees”. All these might contribute to extensive degradation
of the adhesive layer,7,32 but conclusive findings have not
been confirmed. The most recent (to date) one-bottle all-in-
one adhesives appear to be susceptible to phase separation
after dispensing the complex mixture of hydrophobic and hy-
drophilic components,34 and this also is assumed to con-
tribute to bond degradation.33
This study has presented preliminary results of short- and
long-term water storage effects combined with thermocy-
cling for control and 14 all-in-one adhesive/composite treat-
ments. The results show that overall, few if any differences
are found in vitro between the tested products and the ref-
erence materials. Furthermore, based on a quality estimate
associated with the marginal integrity, it has been shown
that early deterioration rates (up to 1 year) can only some-
times be used as estimates for the rate of bond degradation
over a period of 3 years. Indeed, it seems that deterioration
rates due to storage in water are not dependent on the class
(or generation) of the adhesive: large differences in deterio-
ration rates seem to exist between different products, and
these are probably associated with the details of the specif-
ic chemistry. Additional studies are still needed in order to
elucidate to what extent – and in which product – deterio-
ration is critical. These should then be correlated with clini-
cal studies so that decisive conclusions can be drawn .
It appears that the effects of long-term water storage may
not be as detrimental as usually assumed, if indeed the mar-
ginal integrity estimates are appropriate measures of the
quality and effectiveness of recent generations of dental ad-
hesives. A statistically significant decrease in the amount of
MQ1 was only found in 3 out of 14 tested all-in-one adhe-
sives after 1 year water storage. However, in enamel, the
marginal analysis revealed fewer “continuous margins” than
the control groups for G-Bond, AQ Bond, Hybrid Bond, and
One-up Bond F Plus, and this was already observed after 1
year of water storage.
As new results of clinical evaluations emerge, and with a
growing body of data from in vitro measurements, it is hoped
that a clearer understanding of the long-term effects of the
use of these systems will emerge, thus providing an im-
proved guide for clinical judgement.
REFERENCES
1. Anusavice KJ. Criteria for selection of restorative materials: properties ver-
sus technique sensitivity. In: Anusavice KJ (ed). Quality evaluation of dental
restorations. Chicago: Quintessence, 1989:15-56.
2. Armstrong SR, Vargas MA, Fang Q, Laffoon JE. Microtensile bond strength
of a total-etch 3-step, total-etch 2-etch, self-etch 2-step, and a self-etch 1-
step dentin bonding system through 15-month water storage. J Adhes Dent
2003;5:47-56.
3. Armstrong SR, Vargas MA, Chung I, Pashley DH, Campbell JA, Laffoon JE,
Qian F. Resin-dentin interfacial ultrastructure and microtensile dentin bond
strength after five-year water storage. Oper Dent 2004;29-26:705-712.
239
Blunck/Zaslansky
4. Blunck U, Roulet JF. In vitro marginal quality of dentin-bonded composite
resins in Class V cavities. Quintessence Int 1989;20:407-412.
5. Bouillaguet S, Gysi P, Wataha JC, Ciucchi B, Cattani M, Godin C, Meyer JM.
Bond strength of composite to dentin using conventional, one-step, and
self-etching adhesive systems. J Dent 2001;29:55-61.
6. De Munck J, Van Meerbeek B, Satoshi I, Vargas M, Yoshida Y, Armstrong S,
Lambrechts P, Vanherle G. Microtensile bond strengths of one- and two-
step self-etch adhesives to bur-cut enamel and dentin. Am J Dent 2003;
16:414-420.
7. De Munck J, Van Meerbeek B, Yoshida Y, Inoue S, Vargas M, Suzuki K,
Lambrechts P, Vanherle G. Four-year water degradation of total-etch adhe-
sives bonded to dentin. J Dent Res 2003;82:136-140.
8. De Munck J, Van Landuyt K, Peumans M, Poitevin A, Lambrechts P, Braem
M, van Meerbeek B. A critical review of the durability of adhesion to tooth
tissue: methods and results. J Dent Res 2005;84:118-132.
9. Feilzer AJ, De Gee AJ, Davidson CL. Setting stress in composite resin in re-
lation to configuration of the restoratives. J Dent Res 1987;66:1636-1639.
10. Frankenberger R, Krämer N, Petschelt A. Fatigue behaviour of different
dentin adhesives. Clin Oral Invest 1999;3:11-17.
11. Frankenberger R, Perdigão J, Rosa BT, Lopes M. 'No-bottle' vs 'multi-bottle'
dentin adhesives - a microtensile bond strength and morphological study.
Dent Mater 2001;17:373-380.
12. Frankenberger R, Pashley DH, Reich SM, Lohbauer U, Petschelt A, Tay FR.
Characterisation of resin-dentine interfaces by compressive cyclic loading.
Biomat 2005;26:2043-2052.
13. Frankenberger R, Tay FR. Self-etch vs etch-and-rinse adhesives: effect of
thermo-mechanical fatigue loading on marginal quality of bonded resin
composite restoration. Dent Mater 2005;21:397-412.
14. Fritz UB, Finger WJ. Bonding efficiency of single-bottle enamel/dentin ad-
hesives. Am J Dent 1999;12:277-282.
15. Giachetti L, Russo DS, Bertini F, Pierleoni F, Nieri M. Effect of operator skill
in relation to microleakage of total-etch and self-etch bonding systems J
Dent 2006;in press:
16. Hashimoto M, Ohno H, Sano H, Kaga H, Oguchi H. Degradation patterns of
different adhesives and bonding procedures. J Biomed Mater Res
2003;66B:324-330.
17. Heintze SD. The correlation between the evaluation of marginal quality and
bond strength and its clinical relevance – a systematic review. J Adhes
Dent 2007;9(Suppl 1):77-106
18. Henisch G. Ein computergestütztes System zur Erfassung und Verwaltung
von Messdaten im Rahmen der quantitativen Randanalyse am Rasterelek-
tronenmikroskop. Berlin: Free University, 1989.
19. Inoue S, Vargas MA, Abe Y, Yoshida Y, Lambrechts P, Vanherle G, Sano H,
Van Meerbeek B. Microtensile bond strength of eleven contemporary adhe-
sives to dentin. J Adhes Dent 2001;3:237-245.
20. Inoue S, Vargas MA, Abe Y, Yoshida Y, Lambrechts P, Vanherle G, Sano H,
Van Meerbeek B. Microtensile bond strength of eleven contemporary adhe-
sives to enamel. Am J Dent 2003;16:329-334.
21. Jacobsen T, Söderholm KJ. Effect of primer solvent, primer agitation, and
dentin dryness on shear bond strength to dentin. Am J Dent 1998;11:225-
228.
22. Kato G, Nakabayashi N. The durability of a adhesion to phosphoric acid
etched, wet dentin substrates. Dent Mater 1998;14:347-352.
240
23. Kitasako Y, Burrow MF, Nikaido T, Tagami J. Long-term tensile bond durabil-
ity of two different 4-META containing resin cements to dentin. Dent Mater
2002;18:276-280.
24. Peutzfeldt A, Asmussen E. Determinants of in vitro gap formation of resin
composites. J Dent 2004;32:109-115.
25. Retief DH. Do adhesives prevent microleakage? Int Dent J 1994;44:19-26.
26. Roulet JF, Reich T, Blunck U, Noack M. Quantitative margin analysis in the
scanning electron microscope. Scanning Microsc 1989;3:147-158; discus-
sion 58-59.
27. Sano H, Yoshikawa T, Pereira PNR, Kanemura N, Morigami M, Tagami J,
Pashley DH. Long-term durability of dentin bonds made with a self-etching
primer, in vivo. J Dent Res 1999;78:906-911.
28. Sideridou I, Achilias DS, Kyrikou E. Thermal expansion characteristics of
light-cured dental resins and resin composites. Biomat 2004;25:3087-
3097.
29. Sidhu SK, Carrick TE, McCabe JF. Temperature mediated coefficient of di-
mensional change of dental tooth-colored restorative materials. Dent
Mater 2004;20:435-440.
30. Tay FR, Pashley DH, Suh BI, Carvalho RM, Itthagarun A. Single-step adhe-
sives are permeable membranes. J Dent 2002;371-382.
31. Tay FR, Pashley DH, Yoshiyama M. Two modes of nanoleakage expression
in single-step adhesives. J Dent Res 2002;81:472-476.
32. Tay FR, Pashley DH. Water treeing--a potential mechanism for degradation
of dentin adhesives. Am J Dent 2003;16:6-12.
33. Van Landuyt K, De Munck J, Coutinho E, Peumans M, Lambrecht P, Van
Meerbeek B. Bonding to dentin: smear layer and the process of hybridiza-
tion. In: Eliades G, Watts DC, Eliades T (eds). Dental hard tissues and
bonding. Berlin: Springer, 2005:89-122.
34. Van Landuyt KL, De Munck J, Snauwaert J, Coutinho E, Poitevin A, Yoshida
Y, Inoue S, Peumans M, Suzuki K, Lambrechts P, Van Meerbeek B.
Monomer-solvent phase separation in one-step self-etch adhesives. J Dent
Res 2005;84:183-188.
35. Van Meerbeek B, Perdigao J, Lambrechts P, Vanherle G. The clinical perfor-
mance of adhesives. J Dent 1998;26:1-20.
36. Van Meerbeek B, De Munck J, Yoshida Y, Inoue S, Vargas M, Vijay P, Van
Landuyt K, Lambrechts P, Vanherle G. Buonocore memorial lecture. Adhe-
sion to enamel and dentin: current status and future challenges. Oper
Dent 2003;28:215-235.
37. van Meerbeek B, Kanumilli P, de Munck J, Van Landuyt K, Lambrechts P,
Peumans M. A randomized controlled study evaluating the effectiveness of
a two-step self-etch adhesive with and without selective phosphoric-acid
etching of enamel. Dent Mater 2005;21:375-383.
Clinical relevance: Quantitative in vitro long-term mea-
surements of margin integrity help to better understand
the performance of composite resin restorations in the
clinic. In combination with clinical studies this should
provide a deeper understanding of the adhesive failure
an which remains enormous challenge for dentists.
The Journal of Adhesive Dentistry
Clinical Bonding of a Single-step Self-etching Adhesive
in Noncarious Cervical Lesions
Jan WV van Dijkena/Karin Sunnegårdh-Grönbergb/Ebba Sörenssonb

Purpose: The aim of this study was to evaluate the clinical retention to dentin of a single-step self-etching adhesive
system.

Materials and Methods: A total of 133 Class V restorations were placed with the self-etching primer Xeno III and a
resin composite (Tetric Ceram) or a polyacid-modified resin composite (Dyract AP) in noncarious cervical lesions with-
out intentional enamel involvement. The restorations were evaluated at baseline and then every 6 months during a 2-
year follow-up. Dentin bonding efficacy was determined by the percentage of lost restorations.

Results: During the 2 years, 130 restorations could be evaluated. The cumulative loss rate at 2 years was 7.7%, with
no significant differences between the two restorative materials. The self-etching adhesive fulfilled the 18-month full
acceptance ADA criteria.

Conclusion: The single-step self-etching adhesive showed acceptable clinical retention rates to dentin surfaces dur-
ing the evaluation period independent of restorative material used.

Keywords: adhesion, clinical, cervical, dental material, etch, resin, restoration, self-etching.

J Adhes Dent 2007; 9: 241-243. Submitted for publication: 15.12.06; accepted for publication: 8.1.07.

T he introduction of primers containing amphiphilic mono-

mers – dissolved in solvents such as water, acetone, or
alcohol to promote wetting of the dentin and replace water
– changed dentin bonding to a more reliable clinical proce-
dure. These primers infiltrate the nanospaces of the colla-
gen network, caused by the etching procedure, and create
after polymerization an entangled molecular mesh with the
collagen fibrils.4 A high micromechanical bond to the dental
tissue can be obtained by formation of the so-called hybrid
layer. In the multistep etch-and-rinse systems, clinical suc-
cess is partly operator related. The etching and primer ap-
plication steps are critical in this approach. Bonding proce-
a Professor, Department of Odontology, Dental School Umeå, Umeå University,
Umeå, Sweden.
b Assistant Professor, Department of Odontology, Dental School Umeå, Umeå Uni-
versity, Umeå, Sweden.
Paper presented at Satellite Symposium on Dental Adhesives, Dublin,
September 13th, 2006.
Reprint requests: Prof. Jan WV van Dijken, Department of Odontology, Dental
School Umeå, Umeå University , 901 87 Umeå, Sweden. Tel: +46-90-785-6034,
Fax: +46-90-770-580. e-mail: Jan.van.Dijken@odont.umu.se
dures not involving phosphoric acid etching, such as the self-
etching adhesives, were introduced in the 90s to simplify the
adhesive procedure and decrease the technique sensitivity
of the etch-and-rinse systems. The simultaneous self-etch-
ing and primer infiltration makes these systems more user
friendly, eliminating the risk of over etching and over drying.
Today, there are two self-etching systems. The two-step self-
etching adhesives have a separate priming step with more
hydrophilic monomers and a more hydrophobic bonding
step. In the all-in-one or one-step self-etching adhesives, one
liquid containing all the components for etching, priming,
and bonding is applied to the dental tissues. Earlier mild self-
etching adhesives showed etching patterns of the enamel
which were not adequate for clinical retention, and some
manufacturers recommended the adjunctive use of phos-
phoric acid when bonding to enamel.5 Incompatibility with
autocuring resin composites and permeability to water
movement after polymerization have been reported for the
first all-in-one adhesives.14,15 Newer self-etching adhesives
contain more aggressive etchants and showed higher ten-
sile bond strength compared to established dentin bonding
agents.7 The aim of this study was to investigate the clinical
dentin bonding effectiveness of a new one-step self-etching
adhesive in combination with a resin composite material or
a polyacid resin-modified resin composite in noncarious cer-

Vol 9, Supplement 2, 2007 241

van Dijken et al
vical lesions. The hypothesis tested was that the polyacid
resin-modified resin composite would show better clinical re-
tention.
MATERIALS AND METHODS
A total of 133 Class V restorations were placed in 57 patients
(32 men and 25 women) with a mean age of 61.5 years
(range 43 to 84), for whom treatment of noncarious cervical
lesions was indicated. All restorations were placed in dentin
lesions without any intentional enamel involvement, by one
experienced operator familiar with adhesive dentistry. Forty-
four restorations were placed in anterior teeth, 55 in pre-
molars and 32 in molars. Fifty-nine restorations were made
in the maxillary arch and 74 in the mandibular. A single-step
self-etching primer (Xeno III, Dentsply/DeTrey; Konstanz,
Germany; lot nr 0206001237) was evaluated in combina-
tion with two different restorative resinous materials, a hy-
brid resin composite (Tetric Ceram, Ivoclar/Vivadent;
Schaan, Liechtenstein; lot E17820) and a polyacid-modified
resin composite (Dyract AP, Dentsply/DeTrey; batch nr
0203001190). Liquid A of the two-part adhesive system
contains water, ethanol, HEMA, UDMA and BHT (2,6-di-tert-
butyl-p hydroxyl toluene) and nanofiller. Liquid B contains
UDMA, CQ, EPD (p-dimethylaminoethyl benzoate) and two
patented monomers Pyro-EMA (tetramethacryloxyethyl py-
rophosphate and PEM-F (pentamethacryloxyethyl cyclophos-
phazene monofluoride).
The operative field was isolated with cotton rolls and a
saliva suction device. Before conditioning, the lesions were
cleaned of plaque and/or saliva if necessary. The adjacent
gingiva was retracted by gingival retraction instruments or
matrix bands when necessary to secure unrestricted conta-
mination-free access to the field. No bevel was placed. Ap-
plication of the primer was performed according to the man-
ufacturers’ instructions. After mixing, the primer was ap-
plied for 20 s, carefully air dried for some seconds to remove
242
Fig 1 Relative cumulative loss rates
(%) of the Xeno III bonding system in
combination with the two restorative
materials (Tetric Ceram, Dyract AP).
the solvent, taking care not to thin the primer layer. The lay-
er was then light cured for at least 10 s (Astralis 7, HP cur-
ing mode; Ivoclar/Vivadent). Sixty-five restorations were
made at random with the polyacid resin-modified resin com-
posite and 68 with a high-viscosity resin composite restora-
tive material. The restoratives were applied in most cases in
two increments using selected composite instruments (Hu
Friedy; Leimen, Germany) and light cured. All participants
were informed about the material and the follow-up evalua-
tions according to the rules at the Dental School Umeå. The
restorations were evaluated at 6, 12, 18, and 24 months us-
ing slightly modified USPHS criteria.3,5 Only the retention
evaluations are reported here. Postoperative sensitivity was
registered. Descriptive statistics were used to present the re-
sults. Cumulative retention failures were calculated by di-
viding the number of lost restorations at the recalls by the
total number evaluated at the respective recall. Differences
in distribution of the ratings between the adhesive systems
for the investigated variables were statistically analyzed with
the binomial test for independent samples and intraindivid-
ual comparisons of the 2 materials with Friedman’s two-way
analysis of variance.13
RESULTS
At the end of the follow-up, 130 restorations could be eval-
uated. One patient with three restorations was not able to at-
tend the 2-year recall. No recurrent caries was observed or
postoperative sensitivity reported. Ten lost restorations
(7.7%) were observed during the 2-year follow-up, resulting
in relative cumulative failure frequencies for all restorations
at 6, 12, 18, and 24 months of 0.8%, 3.1%, 6.9%, and 7.7%,
respectively. The failure frequencies for the restorations with
Tetric Ceram at the four evaluations were 0%, 0%, 5.9%, and
7.4%, and for Dyract AP restorations 1.6%, 6.5%, 8.1%, and
8.1%, respectively; the differences were not statistically sig-
nificant (Fig 1).
The Journal of Adhesive Dentistry

DISCUSSION
The rapid progression of adhesive materials during the last
20 years has resulted in a situation where many adhesive
systems have been replaced by modified successors which
were claimed to be better without clinical validation. Clinical
trials have been limited in number since they require sever-
al years of regular recalls. Enamel-resin bonds produced af-
ter acid etching with phosphoric acid have proven satisfac-
tory and stable over time.2,5,6 Adhesion to dentin, on the oth-
er hand, has been difficult to achieve because of the sub-
strate’s wet nature. The efficacy of dentin bonding can be
demonstrated in cervical abrasion/erosion lesions without
involvement of the contiguous enamel. These surfaces are
ideal to test clinical dentin bonding because they are wide-
ly available.12 Therefore, no enamel bevel was made in the
study and care was taken not to involve the enamel surface
contiguous with the lesions during the etching-priming step.
However, many of the lesions still contained a small enam-
el margin in the incisal area, and the evaluation of clinical
retention to only dentin tissue was therefore not 100%. At
the end of the two years, the recall rate was high (130/133).
The retention rate for the adhesive system was 92.3%.
Türkün recently reported a 96% retention rate after one year
for the same adhesive.16 For provisional acceptance, the lat-
est guidelines of the American Dental Association (Dental
and enamel adhesive materials: ADA, Council on Dental Ma-
terials, Instruments, and Equipment, 1994) for submission
of dentin and enamel adhesive materials require that no
more than 5% of the restorations have been lost and not
more than 5% of the restorations may show microleakage at
the 6-month recall. To obtain full acceptance, the cumulative
incidence of clinical failures in each of two independent clin-
ical studies has to be lower than 10% lost restorations and
10% microleakage after 18 months. The dentin retention
rates for the tested adhesive were 3.1% and 6.9% at 6 and
18 months, respectively, fulfilling the ADA guidelines for
enamel-dentin adhesive systems. There were no significant
differences in clinical retention rates between the restora-
tions placed with the resin composite or the polyacid-modi-
fied resin composite. The hypothesis was therefore not ac-
cepted. Kemp-Scholte et al8 showed that materials with low-
er elasticity modulus can act as an elastic buffer, which re-
lieved contraction stresses and improved marginal integrity.
Since most polyacid-modified resin composites include
resins with a modulus of elasticity value between those of
resin composite and glass-ionomer cement, these materials
may work as a stress-breaking barrier between the tooth and
the composite.1 A significantly better adaptation was ob-
served with the SEM replica technique for a polyacid-modi-
fied resin composite/resin composite sandwich technique
compared to resin composite only restorations.9 However,
the same authors could not show any clinical evidence for
the interfacial adaptation results observed by SEM. No sig-
nificant statistical or clinical differences were observed be-
tween the two techniques during 3- and 9-year periods.10,11
The polyacid-modified resin composite tested in the present
study has a modulus of elasticity value close to that of resin
Vol 9, Supplement 2, 2007
van Dijken et al
composite materials, which may partly explain why no dif-
ferences were observed (personal communication, E. As-
mussen).
CONCLUSION
It can be concluded that the single-step self-etching adhe-
sive showed acceptable clinical retention rates during the
evaluation period, independent of restorative material used.
ACKNOWLEDGMENTS
This study was supported in part by the County Council of Västerbotten
and Dentsply DeTrey, Konstanz, Germany.
REFERENCES
1. Attin T, Vataschki M, Hellwig E. Properties of resin-modified glass-ionomer
restorative materials and two polyacid-modified resin composite materials.
Quintessence Int 1996;27:203-209.
2. de Munck J, van Landuyt K, Peumans M, Poitevin A, Lambrechts P, Braem M,
van Meerbeek B. A critical review of the durability of adhesion to tooth tis-
sue: methods and results. J Dent Res 2005;84:118-132.
3. Dijken van JWV. A clincial evaluation of anterior conventional, microfiller and
hybrid composite resin fillings. A six year follow up study. Acta Odont Scand
1986;44:357-367.
4. Dijken van JWV. Multi-step versus simplified enamel-dentin bonding systems-
Réalités Cliniques 1999;10:199-222.
5. Dijken van JWV. Durability of new restorative materials in Class III cavities. J
Adhes Dent 2001;3:65-70.
6. Frankenberger R, Krämer N, Petschelt A. Long term effect of dentin primers
on enamel bond strength and marginal adaptation. Oper Dent 2000;25:11-
19.
7. Gernhardt CR, Biesecke G, Schaller HG. Tensile bond strength of a self-con-
ditioning dentin adhesive system in vitro [abstract 338]. J Dent Res
2003;82:B 55.
8. Kemp-Scholte CM, Davidson CL. Marginal integrity related to bond strength
and strain capacity of composite resin restorative systems. J Prosth Dent
1990;64:658-664.
9. Lindberg A, Dijken van JWV, Hörstedt P. Interfacial adaptation of a Class II
polyacid-modified resin composite/ resin composite laminate restoration in
vivo. Acta Odont Scand 2000;58:77-84.
10. Lindberg A, van Dijken JWV, Lindberg M. A 3-year evaluation of a new open
sandwich technique in class II cavities. Am J Dent 2003;15:33-36.
11. Lindberg A, van Dijken JWV, Lindberg M. 9-year evaluation of a poly-acid-mod-
ified resin composite open sandwich technique in class II cavities. J Dent
2007;35:124-129.
12. Peumans M, Kanumilli P, De Munck J, van Landuyt K, Lambrechts P, van
Meerbeek B. Clinical effectiveness of contemporary adhesives: A systemat-
ic review of current clinical trials. Dent Mater 2005;21:864-881.
13. Siegel S. Nonparametric Statistics. New York: McGraw-Hill, 1956.
14. Tay FR, Pashley DH. Water-treeing – a potential mechanism for degradation
of dentin adhesives. Am J Dent 2003;16:6-12.
15. Tay FR, Pashley DH, Yiu CKY, Sanares AME, Wei SHY. Factors contributing to
the incompatibility between simplified-step adhesives and self-cured or dual-
cured composites. Part I. Single-step self-etch adhesive. J Adhes Dent
2003;5:27-40.
16. Türkün LS. The clinical performance of one- and two-step self-etching adhe-
sive systems at one year. J Am Dent Assoc 2005;136:656-664.
Clinical relevance: The adhesive showed a good clinical
performance during the 2 year follow-up in noncarious cer-
vical lesions.
243
Sarrett

244 The Journal of Adhesive Dentistry

Shear Bond Strength and Physicochemical Interactions
of XP Bond
Mark A. Lattaa

Purpose: The purpose of this study was to evaluate the shear bond strength of composite to dentin and enamel using
the new etch-and-rinse adhesive XP Bond compared to other adhesives (Optibond Solo Plus, Apder ScotchBond 1 XT,
Syntac Classic).

Materials and Methods: Shear bond strength (MPa) was measured by shearing a resin cylinder 4.5 mm in diameter
from prepared buccal surfaces of human third molars using an Instron Testing Machine equipped with a chisel-
shaped rod. In addition, micro-Raman spectroscopy was performed to determine if there was a chemical interaction
between the resin adhesive and dentin and enamel.

Results: Significant differences were observed among the dentin and enamel values generated with the adhesives
tested. XP Bond generated statistically similar values to Optibond Solo Plus and Apder ScotchBond 1 XT to both
enamel and dentin. Syntac Classic generated significantly lower values to both enamel and dentin.

Conclusion: Micro-Raman spectroscopy showed a complete infiltration of resin into the demineralized dentin zone. In
addition, it strongly suggested a chemical interaction with XP Bond and components of dentin. It is hypothesized that
this interaction is due to the formation of calcium phosphate complexes derived from mineral apatite in the dentin
and phosphate esters in the adhesive.

Keywords: adhesion, bonding, chemical analysis, Raman spectroscopy.

J Adhes Dent 2007; 9: 245-248. Submitted for publication: 15.12.06; accepted for publication: 11.1.07.

I n spite of significant improvements in dental adhesives in

the last decade, achieving a durable bond and seal of
resin based restorative materials still remains a challenge.
The primary mechanism for bonding to dentin with etch-and-
rinse adhesives is via the removal of the dentin smear layer
and surface mineral followed by infiltration and entangle-
ment of resin monomers into the exposed collagen matrix in
the demineralized zone.2 This resultant mixture of resin, col-
lagen, and mineral is termed the hybrid zone.4 The exposed
collagen fibrils are suspended in water, creating space for
a Associate Dean for Research, Professor of General Dentistry, Creighton Uni-
versity School of Dentistry, Omaha NE, USA.
Paper presented at Satellite Symposium on Dental Adhesives, Dublin,
September 13th, 2006.
Reprint requests: Prof. Mark A. Latta, D.M.D., M.S., Associate Dean for Re-
search, Professor of General Dentistry, Creighton University School of Dentistry,
2500 California Plaza, Omaha NE 68178, USA. Tel: +1-402-280-5044, Fax: +1-
402-280-5004. e-mail: mlatta@creighton.edu
the penetration of the resin monomers. Drying collagen re-
sults in its collapse and may prevent full infiltration of the ad-
hesive resin.3 Clinically, it is difficult to create the optimal
dentin moisture for bonding. However, failure to do so may
lead to postoperative sensitivity, bond failure, leakage, and
ultimately early failure of the restoration.
There are numerous in-vitro testing methods to evaluate
the properties of resin adhesives. While bond strength test-
ing does not definitively predict clinical behavior, compari-
son of new systems with adhesives of known clinical perfor-
mance can yield valuable information.1,5,9 Microscopically,
the interfacial interaction between adhesive and tooth struc-
ture is typically investigated with scanning electron mi-
croscopy and transmission electron microscopy. However,
there is only limited chemical structural investigation of the
resin/tooth interface. The minimal thickness of the
tooth/adhesive interface requires an analytical technique
with very high resolution. Micro-Raman spectroscopy has
been shown to be a very promising technique for investigat-
ing the adhesive bond with tooth structure.7,8,10,11 It has nu-
merous advantages, including the ability to analyze speci-

Vol 9, Supplement 2, 2007 245

Latta
Table 1 Mean shear bond strength (SBS) for each group (in MPa)
Bonding Agent Mean SBS to dentin (MPa)
Optibond Solo plus 26.5 ± 2.9
XP Bond 25.8 ± 2.6
Adper Scotchbond 1 XT 24.2 ± 3.4
Syntac Classic (15-s etch) 13.2 ± 3.7*
* Significantly different compared to the other groups (p < 0.05)
mens in air or water, at room temperature and pressure, and
without destroying the specimen.
A new etch-and-rinse adhesive called XP Bond has been
developed that has several unique compositional compo-
nents. It is hypothesized that these components will allow
the adhesive formula to be less sensitive to residual dentin
moisture and allow full resin penetration under a wide range
of dentin conditions. Second, this adhesive contains phos-
phate esters that may chemically interact with the mineral
apatite component of dentin and enamel. The purpose of
this study was to evaluate the shear bond strength of com-
posite to dentin and enamel using this new adhesive system.
In addition, micro-Raman spectroscopy was performed to
determine if there was a chemical interaction between the
resin adhesive and dentin and enamel.
MATERIALS AND METHODS
Shear Bond Strength
Flat bonding sites were prepared on the buccal surfaces of
96 extracted human teeth by grinding the teeth on a water-
cooled abrasive wheel (Ecomet III Grinder, Lake Bluff, IL,
USA) to a 600-grit surface exposing dentin on 48 specimens
and enamel on 48 specimens. Twelve specimens each for
enamel and dentin for each adhesive were prepared. The ad-
hesives and conditions of use were:
• Group 1: XP Bond (lot 0503004020) cured for 10 s with
the SmartLite LED curing light.
• Group 2: Optibond Solo Plus (lot 437041) cured for 10 s
with the SmartLite LED curing light.
• Group 3: Adper Scotchbond 1 XT (lot 230270) for 10 s
with the SmartLite LED curing light.
• Group 4: Syntac Classic (lot G06551) using phosphoric
acid etch 15 s and cured for 10 s with the SmartLite LED
curing light.
DeTrey tooth conditioner (Dentsply Detrey; Konstanz, Ger-
many; lot 0403000687) was used to condition all surfaces
prior to placement of the adhesive. After the application of
the adhesive system, cylinders of composite resin (Spectrum
TPH Shade A2, lot 0411002236; Dentsply DeTrey; Kon-
stanz, Germany) were bonded to each dentin and enamel
bonding site. A gelatin capsule technique in which a resin
cylinder 4.5 mm in diameter is employed as a matrix was
246
Mean SBS to enamel (MPa)
28.3 ± 4.8
28.3 ± 4.7
26.5 ± 4.9
21.6 ± 5.8*
used. Composite was loaded in the capsules approximately
two-thirds full, then cured in a Triad 2000 curing unit (Trubyte
Division, DENTSPLY International; York, PA, USA) for 1 min.
Additional composite was added to slightly overfill the cap-
sules. The capsules were firmly seated against the bonding
sites and excess resin removed with a dental explorer. The
resin was visible-light cured with three 20-s curing se-
quences, each from opposite sides of the capsule at an an-
gle of 45 degrees to the tooth surface.
The specimens were stored in distilled water at 37°C for
24 h. Twelve specimens for each adhesive/tooth structure
combination were thermocycled between water baths of 5°C
and 55°C for 6000 cycles (dwell time 20 s). The specimens
were mounted in acrylic and loaded to failure in an Instron
Testing Machine (Model 1123, Instron; Canton, MA, USA)
equipped with a chisel-shaped rod. Each bonded cylinder
was placed under continuous loading at 5 mm per min un-
til fracture occurred. Shear bond strength was calculated in
MPa.
Raman Spectroscopy
Extracted third molars were prepared by grinding enamel
and dentin to a 600-grit surface. The experimental adhesive
was applied and composite resin placed over the adhesive
film. After water storage, the teeth were sectioned to expose
the tooth/adhesive interface and polished to 4000 grit with
silicon carbide paper. Specimens were placed on an X-Y
scanning stage in a Jasco 3100 laser Raman Spectrometer
(Jasco; Tokyo, Japan). The excitation was derived from a
785-nm source at an output level of 35 mW and focused
through an X100 near-IR lens to ~1 μm beam diameter.
Wavenumber calibration was determined by comparison of
spectra from pure silicon (520 cm-1).
RESULTS AND DISCUSSION
Shear Bond Strength
The mean shear bond strength (in MPa) for each group is dis-
played in Table 1. A one-way ANOVA was done for the dentin
and enamel groups. The level of significance for dentin was
p < 0.0001, and for enamel p = 0.0168. A post-hoc LSD test
was done for pair-wise comparison. The group marked by an
asterisk was statistically different compared to the other
groups (p < 0.05).
The Journal of Adhesive Dentistry

Fig 1 Representative spectra of dentin (left) and dentin impregnated with XP Bond (right). Circle represents peak shift and broadening in
the 1100 to 1170 cm-1 range is suggestive of calcium-phosphate ester complex formation.
Fig 2 Representative spectrum of XP Bond showing major func-
tional groups. Plot of peak intensity vs wavenumber cm-1.
Raman Spectroscopy
A representative spectrum of XP Bond is shown in Fig 1. Rep-
resentative Raman spectra of human dentin and resin im-
pregnated dentin with XP Bond are shown in Fig 2. The most
intense band occurs at 960 cm-1 and is associated with the
P-O stretch of the phosphate in the mineral apatite. Also ob-
served are bands at 1245 cm-1 (amide III) and 1667 cm-1
(amide I) associated with collagen. The mixture shown on the
right clearly shows the apatite and amide I peaks mixed with
features only associated with the adhesive. The peak shift
and broadening in the 1100 to 1170 cm-1 area is not seen
in the pure dentin or XP Bond spectrum, and is associated
with the formation of calcium/phosphate ester complexes in
the hybrid layer.6
The relative peak intensities of the mineral apatite (960
cm-1), resin carbonyl (1720 cm-1), collagen (1670 cm-1), and
phosphate complex (centered at 1146 cm-1) were plotted
across the dentin interface and are shown graphically in
Vol 9, Supplement 2, 2007
Latta
Fig 3 Peak intensity for characteristic marker peaks for dentin,
mineral and resin are plotted across the dentin/adhesive inter-
face. The resin peak at 1720 cm-1 fully penetrates to the bottom
of the demineralized zone. In addition, the maximum strength of
the 1146 cm-1 peak is offset from the resin, indicating an interac-
tion with components in the dentin layer.
Fig 3. The strength of the phosphate complex intensity in the
intermediate hybrid layer is strongly suggestive of a chemi-
cal interaction between components in the resin adhesive
and the dentin. In addition, the resin is fully penetrated to
the depth of the zone of demineralization.
CONCLUSION
Significant differences in shear bond strength were ob-
served among the dentin and enamel values generated with
the adhesives tested. XP Bond generated statistically simi-
lar values to Optibond Solo Plus and Apder ScotchBond 1 XT
to both enamel and dentin. Syntac Classic generated signif-
icantly lower values to both enamel and dentin.
Micro-Raman spectroscopy showed a complete infiltra-
tion of resin into the demineralized dentin zone. In addition,
it strongly suggested a chemical interaction with XP Bond
247
Latta
and components of dentin. It is hypothesized that this inter-
action is the formation of calcium phosphate complexes de-
rived from mineral apatite in the dentin and phosphate es-
ters in the adhesive.
ACKNOWLEDGMENTS
This research was partly sponsored by Dentsply DeTrey, Konstanz,
Germany.
REFERENCES
1. Barkmeier WW, Hamesfahr PD, Latta MA. Bond strength of composite to
enamel and dentin using Prime and Bond 2.1. Oper Dent 1999;24:51-56.
2. Eick JD, Gwinnet AJ, Pashley DH, Robinson SJ. Current concepts in adhe-
sion to dentin. Crit Rev Oral Biol Med 1997;8:306-335.
3. Gwinnett AJ. Quantitative contribution of resin infiltration/hybridization to
dentin bonding. Am J Dent 1993;6:7-9.
4. Nakabayashi N, Kijima K, Masuhara E. The promotion of adhesion by the
infiltration of monomers into tooth substrates. J Biomed Mater Res
1982;16:265-273.
5. Naughton WT, Latta MA. Bond strength of composite to dentin using self-
etching adhesive systems. Quintessence Int 2005;36:41-44.
248
6. Penel G, Leroy N, Rey C, Lemaitre J, Van Landuyt P, Ghanty N. Qualitative
and quantitative investigation of calcium phosphate of biological interest
by Raman micro-spectrometry. Recent Res Develop Appl Spectroscopy
1999;2:137-146.
7. Sato M, Miyazaki M. Comparison of depth of dentin etching and resin infil-
tration with single-step adhesive systems. J Dent 2005;22:475-484.
8. Spencer P, Wang Y, Walker MP, Wieliczka DM, Swafford JR. Interfacial
chemistry of the dentin/adhesive bond. J Dent Res 2000;79:1458-1463.
9. Shaddy RS, Latta MA, Goren M. The effect of salivary contamination on ad-
hesive shear bond strength. J Pract Hygiene 2003;12:27-28.
10. Wang Y, Spencer P. Hybridization efficiency of the adhesive dentin inter-
face with wet bonding. J Dent Res 2003;82:141-145.
11. Wang Y, Spencer P. Physicochemical interactions at the interface between
self-etch adhesive systems and dentine. J Dent 2004;32:567-579.
Clinical relevance: The laboratory bond values for a
newly developed etch and rinse adhesive system would
suggest exellent clinical performance. The discovery of
chemical interaction between the adhesive and the min-
eral component of tooth structure may help explain the
high bond strengths and also might predict the genera-
tion of a stable long term bond interface clinically.
The Journal of Adhesive Dentistry
Microshear Fatigue Testing of Tooth/Adhesive
Interfaces
Marc Braema

Purpose: The objective of the present study was to determine the fatigue resistance of several contemporary dentin
adhesives as well as a resin-modified glass-ionomer cement.

Materials and Methods: Cyclic loading of the adhesive interface was achieved by a microshear fatigue setup follow-
ing a staircase approach, where the stress level at which 50% of the specimens fail after 104 cycles was calculated
as the median microshear fatigue resistance (μSFR).

Results: For all products tested, the μSFR was lower than the microshear strength. A wide spread in μSFR was ob-
served, ranging from 24% to 76% of the quasi-static microshear strength, irrespective of the type of adhesive used.

Conclusion: The results of this study show that the microshear test setup is a discriminative and reproducible way of
testing tooth/adhesive interfaces, even at relatively low stresses. The results clearly indicate that such interfaces are
vulnerable to progressive damage by cyclic loads. Further, at present there is not one bonding approach, whether
“total etch” or “self-etching”, that consistently yields higher fatigue resistance: the product factor seems to be of pri-
mary importance.

Keywords: fatigue, dental adhesive, dynamic testing.

J Adhes Dent 2007; 9: 249-253. Submitted for publication: 15.12.06; accepted for publication: 5.1.07.

T he success of bonding restorative materials to tooth tis-

sue is generally expressed as a statically or quasi-stati-
cally determined strength value. Under clinical circum-
stances, however, tooth-restorative bonds are subjected to
cyclic loads that could well induce failure at stress levels sig-
nificantly lower than the ultimate bond strength, a phenom-
enon defined as fatigue.1 In addition, under fatigue condi-
tions, the influence of imperfections in the adhesive inter-
face is more clearly revealed.7 At present, research on
dentin bonding is, among other things, focused on reducing
the number of application steps in the bonding procedure,
thereby assuming a reduction in the risk of defects. In vitro
a Professor, Head of Lab Dental Materials, University of Antwerpen, Antwerpen,
Belgium.
Paper presented at Satellite Symposium on Dental Adhesives, Dublin,
September 13th, 2006.
fatigue testing of these interfaces could therefore better al-
low studying these effects.
Hence, the objective of this study was to determine the
fatigue resistance of several contemporary dental adhesives
and a resin-modified glass-ionomer cement bonded to
dentin, using a custom-built microshear fatigue testing de-
vice.
MATERIALS AND METHODS
Materials
The materials used are shown in Table 1. All tests were per-
formed prior to the expiration date mentioned in the table.
The composite restorative used with dentin bonding was
Clearfil AP-X (Universal Shade A3, Lot 1043 BA; Kuraray,
Japan). All applications were performed as per manufactur-
er’s instructions.

Reprint requests: Dr. Marc Braem, Lab Dental Materials, Groenenborgerlaan

Dentin Specimen Preparation
171, B-2020 Antwerpen, Belgium. Tel: +32-3-265-32-66, Fax: +32-3-265- Dentin collected after extraction of human third molars was
36.35. e-mail: marc.braem@ua.ac.be used. The teeth were stored immediately in chloramine 0.5%

Vol 9, Supplement 2, 2007 249

Braem

at 5°C prior to cutting, which was done within 30 days after

extraction.
After removal of the roots and pulp tissue, the teeth were
Exp Date

2009-01
glued on a cubic clamp and a first cut (Microslice 2, Metals
Research; Cambridge, UK) was made parallel to the occlusal
Light-curing resin

surface to remove the occlusal enamel. Next, the clamp was

rotated 90 degrees and a first series of parallel cuts 3 mm
apart was made perpendicular to the surface. The clamp
G03430

was then again rotated 90 degrees and a new series of cuts

Batch

was made in an identical way. As a result, cubic samples are

created that are broken off the remains of the tooth in order
to make sure that perpendicularly cut tubules will be used
in the test.
2006-08
2005-06

2008-02
2008-02

2005-12

2005-09
2006-06
2008-08
Exp Date

2005-11

2005-11
2005-01

2007-02

2007-11

The dentin cube was then positioned in the center of the

base of the test jig with the test surface against a Plexiglas
plate (Fig 1), immobilized by slight pressure. A light-curing
glass-ionomer cement (Fuji II LC capsules, GC Europe; Haas-
Adhesive

rode, Belgium) was mixed for 10 s followed by 3 s in a Ro-

4AG 20040424

toMix device (3M ESPE; Seefeld, Germany), applied without

0503000835

0512000738
503004020

prior conditioning of the dentin, and light cured for 20 s each

0406161

at the bottom and top surfaces using a QTH light source

G04548
402145

175425

010082
301241

3-1325

61112
41460

(Luxor, ICI; Manchester, UK) with an output of at least 520

Batch

mW/cm2. Output was checked with a radiometer (Optilux

Model 100, SDS Kerr; Danury, CT, USA).
The dentin test surface was prepared using a small piece
of 600-grit grinding paper, cleaned with compressed air and
2006-05
Exp Date

2006-01

water, and thereafter visually inspected under a light micro-

scope. The test surface was then treated according to the
Primer

manufacturer’s instructions for the respective materials.

When separate acid etching was required, a phosphoric acid
gel was used (Scotchbond etching gel, 3M ESPE), except
403204
G01297

when a proprietary etchant is included with the adhesive, as

Batch

is the case for Prime & Bond NT. Polyacrylic acid (GC Condi-
tioner, GC Europe) was used in case of the resin-modified
glass-ionomer cement.
1 step SE 2 components
1-step SE 2 components

Once the final adhesive layer was finished for the dentin
1 step SE 1 component
1 step SE 1 component
glass-ionomer cement
3-step etch and rinse

3-step etch and rinse

3-step etch and rinse
2-step etch and rinse
2-step etch and rinse
2-step etch and rinse

bonding, or the dentin was conditioned prior to the applica-

tion of the resin-modified glass-ionomer cement, a perfo-
rated (diameter 1 mm) Mylar strip (0.05 mm thick) was ac-
curately centered on top of the prepared sample and the up-
2-step SE
2-step SE

per part of the test jig was fixed (Fig 2). A first portion of the
restorative was applied without touching the cavity walls and
Type

light cured. Next the remainder of the cavity was filled and
cured incrementally.
The test jig was then transferred to the fatigue machine
Dentsply DeTrey
Dentsply DeTrey
Dentsply DeTrey

Heraeus-Kulzer

and the screws removed (Fig 3). This method prevents the
Manufacturer

adhesive interface from being unintentionally touched or

GC Europe

GC Europe
3M ESPE

3M ESPE

loaded by any means prior to testing.

Vivadent

Kuraray
Kuraray
Kerr
Kerr

Fatigue Testing
The present method is a modification of a previously de-
Table 1 Materials used

scribed setup.2 All testing was carried out at 35°C under

Adper ScotchBond 1 XT

load-controlled conditions, at a test frequency of 2 Hz.

Clearfil Protect Bond

Adper Prompt-L-Pop

First, the quasi-static microshear strength (τ) was deter-

Optibond Solo Plus
Fuji II LC Capsules

Prime & Bond NT

Clearfil SE Bond

mined by measuring the maximal force at failure divided by

the bonding surface area, which was measured under a light
Brand name

Optibond FL

microscope prior to testing.

XP Bond

G-Bond
Xeno III
Syntac

During the fatigue test, the specimens were subjected to

iBond

cyclic loading. Tests were conducted sequentially, with the

initial stress set at about 50% of the microshear strength of

250 The Journal of Adhesive Dentistry

 Braem

Fig 1 Positioning of the dentin sample with the surface to be Fig 2 Top view of the test jig after preparation of the bond and
tested oriented downwards on a Plexiglas plate. placement of the perforated Mylar strip. The upper part of the jig
is fixed prior to the application of the restorative material.

the adhesive maximum and stressed until failure or 104 cy-

cles. The applied stress in each succeeding test was in-
creased or decreased by a fixed increment of stress, ac-
cording to whether the previous test resulted in failure or no
failure, also described as a staircase approach.6 This fixed
increment is based on pilot testing and fixed at 8% of the mi-
croshear strength.
The results of the fatigue test were analyzed using logis-
tic regression4 to determine the load at which 50% of the
specimens fail, further referred to as the “median micro-
shear fatigue resistance” or μSFR. To compare the fatigue
data obtained from the different experimental groups, a mul-
tiple logistic regression analysis was conducted (Statistica
6.0, StatSoft; Tulsa, OK, USA).

RESULTS
The microshear strength and the μSFR for each material are
given in Table 2. The μSFR was about 43% lower than the re-
spective microshear strength value (Table 2), ranging from
24% in the case of Optibond Solo Plus and iBond, up to 76%
for Clearfil Protect Bond.
Comparing the slope β1 obtained from the logistic regres-
sion (Table 2), a very steep curve can be seen for Xeno III
(β1 = 6.5079) and Adper Prompt-L-Pop (β1 = 5.8161), being
almost 10 times steeper than that of the other resin bonding
agents. In Xeno III, failures were noted after 145, 915, 196,
565, 645, 1465 and 460 cycles and after 245, 1625, 150,
1080, 550, 3595 and 270 cycles for Adper Prompt-L-Pop.
The same can be said, although to a lesser degree, of Fuji II
LC (β1 = 1.1195) with failures at 75, 30, 65, 185, 55, 6750,
40, 565, 7540, 50, and 80 cycles. G-Bond on the other hand
shows a rather flat curve with β1 = 0.1652, with failures not-
ed at 65, 130, 135, 4430, 9475, 260, 55, and 155 cycles.
Using the results from the logistic regression, the 25%
Fig 3 Placement of the test jig in the fatigue machine. The jig is
fixed using compressed air (1). The piezo-electric force transduc-
ers (2) record the applied loads.
and 75% quartiles can be calculated, giving an indication of
the range of the results around the μSFR (Table 2). Com-
paring the different adhesives using multiple logistic re-
gression, the bond strength in MPa (p < 0.0001) as well as
the adhesive (p = 0.0003) contribute significantly to the
model.
DISCUSSION
The lack of fatigue data in the dental literature on adhesive
interfaces is profound. Only some data are available to-
day,4,5,7,10,12,13 in spite of the necessity to complete the qua-
si-static bond strength tests with clinically relevant dynamic
fatigue data. A prerequisite is that the setup is of clinical rel-

Vol 9, Supplement 2, 2007 251

Braem

evance. Assuming 3 periods of 15 min of chewing per day

τ/μSFR

at a chewing rate of 1 Hz, the number of chews is 2700 per

(%)

55

28
30

65
39
52
35

55
42
24

24
76
41
day.14 This amounts to roughly 106 times per year. At this fre-
quency, a fatigue test on 1 sample takes about 12 days to
accomplish 106 cycles. Increasing the rate to 2 Hz will offer
p-value2

0.0000
0.0000
0.0000

0.0000
0.0585

0.0585

0.0003
0.5672
0.0001
0.3987

0.0073

0.0318
0.1056

1) β0 and β1 are parameters of the logistic regression function, determining the probability of failure in terms of stress applied to the interface (S): Y = exp(β0 + β1 •S) / (1 + exp(β0 + β1 •S))
a time-saving approach well within the frequency depen-
dency range of the tested visco-elastic materials. Further-
more, if the noncontact events are eliminated from the
chewing cycles, it can be calculated that 104 cycles repre-
sents about 1.2 months of continuous real-life contact. This
0.5492
0.2893

0.4895

0.3042
0.2991
0.3081

6.9613
0.5188

0.2577

0.1625
1.1195

0.2491

5.1610 approach is justified, since restorations tend to fail either

β11

early, before 104 cycles, or very late, after 105 cycles.9 More-
over, a test run on a sample that does not fail now takes
about 1.5 h to complete, as opposed to about 1 week for
106 cycles.
-4.5580
-16.6834

-2.4908
-4.9682

-8.7526

-132.0255
-175.7207
-6.1994

-9.3190

-3.7347
-5.3315
-9.7454
-4.5571
β01

A common standard in the analysis of fatigue data is the

value at which 50% of the specimens fail after a pre-set num-
ber of cycles.2,4,5 However, in the present type of fatigue test-
ing, considerable errors can be made as to the determination
of the so-called pre-set stress levels due to geometry errors.4
Therefore, the probability of failure at each applied stress lev-
el was approximated by logistic regression where the μSFR
quartile
75%

32.4

22.7
33.8

24.9
36.3
25.4
22.9

15.9
21.0
5.1

14.1

22.1
20.1

represents the value at which 50% of the specimens fail. Cal-

culating the 25% and 75% quartiles further illustrates the
distribution of the obtained data (Table 2). It can be seen
from these data that the products with the steepest slopes
(β1) show the lowest distribution around the μSFR.
quartile
25%

9.7

8.5
28.4
13.4

13.9
26.7
15.7
16.4
28.9

22.5

8.7
3.1

25.1

Some of the adhesives therefore show a so-called type 2

fatigue behavior10 and appear to have a rather well-defined
fatigue stress level or threshold above which they fail rapid-
ly and below which they will survive (Xeno III, Adper Prompt-
L-Pop, Fuji II LC). In other products, such as G-Bond, the op-
μSFR

15.3
30.4

18.3
30.3

20.7

25.2
32.6

22.7

12.3
11.9
4.1

17.2

17.9

posite behavior is found and a wide spread of data around

the μSFR can be noted. Most of the materials show a mixed
Table 2 Results for the microshear strength (τ, MPa) and μSFR (MPa)

type of behavior, indicating that imperfections and defects

probably determine the actual lifespan of the adhesive
bond. Fractographic analysis needs to be carried out to test
this hypothesis.
SD

10.5

3.7
8.3
3.2

2.7
2.0
4.8

3.5
8.4
12.3

10.7
3.1
5.1

The main advantage of the present method is that with

the same setup, both shear strength and fatigue resistance
can be measured and compared. It is also advantageous
that the method requires no processing of the sample once
±

±
±

±
±
±

±
±
±

the interface has been formed, thereby avoiding operator-in-

2) p-value of estimate of the multiple logistic regression

duced defects. The results show that the μSFRs are consis-
tently lower than the respective microshear strength for the
strength
μ-shear

same adhesive (Table 2). This is not surprising, since it is

46.2

54.9
55.5
56.9
49.2

56.4

35.0
42.8

53.5

51.0
51.7
10.1

47.0

known that internal interfacial defects and imperfections

shorten the lifespan of a joint under cyclic fatigue. Hence,
fatigue data generally vary substantially more than static
bond strengths.8 The present results, however, show in
some cases that the variation in the fatigue data is lower
than that present in the quasi-static data, thereby empha-
Adper ScotchBond 1 XT

sizing the need for nontraumatic sample preparation.

Clearfil Protect Bond

Adper Prompt-L-Pop
Optibond Solo Plus

It is beyond the scope of the present article to discuss in

Prime & Bond NT

Clearfil SE Bond

full the possible mechanism of each individual adhesive re-

Fuji II LC Caps
Brand name

Optibond FL

lated to the measured μSFR. The present results emphasize

that within each type of adhesive, products exist that show
XP Bond

G-Bond
Xeno III
Syntac

iBond

a high fatigue resistance. Furthermore, some few-step ad-

hesives perform better than other multi-step ones, while for
others it is just the opposite. Thus, not only the reduction in

252 The Journal of Adhesive Dentistry


the number of steps but also the degree of difficulty of the
step appears to be of primary importance.
The present results indicate that the fatigue behavior of
each individual adhesive must be carefully studied, since
within each group results can be found that outperform
and/or are similar to results obtained by particular adhe-
sives in other groups. This indicates that, in general, the dif-
ferent types of bonding approaches converge to adequate
results. In this context, the result for the glass-ionomer ce-
ment is surprising: both the microshear bond strength and
the μSFR are among the lowest measured in this study. This
can be explained by a mismatch in the mechanical proper-
ties of the glass-ionomer matrix and the glass particles,
causing large stresses to accumulate at their interface.11
However, the clinical performance of these materials under
the right indications is still remarkably good, thus support-
ing the hypothesis that “self-healing” or “repair” might be
possible in glass-ionomer cements,3 although such “heal-
ing” may rather be retardation in crack growth or a crack
growth toughening mechanism due to the plasticizing effect
of the resinous component.
CONCLUSION
Tooth/adhesive interfaces suffer from the progressive dam-
age induced by subcritical cyclic loads. The differing ap-
proaches to achieving tooth-resin bonding are not consis-
tently reflected in differences in fatigue resistance.
ACKNOWLEDGMENTS
The author thanks the manufacturers for the generous donation of ma-
terials. Thanks also to Dr. Jan De Munck, Leuven BIOMAT Research
Cluster K.U. Leuven, Belgium, the statistical analysis could be per-
formed. Finally, the supporting efforts and constructive criticism of Mr.
Geert Keteleer, Lab Dental Materials – Universiteit Antwerpen, are
greatly acknowledged.
This research was partly sponsored by Dentsply DeTrey, Konstanz,
Germany.
Vol 9, Supplement 2, 2007
Braem
REFERENCES
1. Baran GR, Boberick KG, McCool JI. Fatigue of restorative materials. Crit
Rev Oral Biol Med 2001;12:350-360.
2. Braem M, Davidson CL, Lambrechts P, Vanherle G. In vitro flexural fatigue
limits of dental composites. J Biomed Mater Res 1994;28:1397-1402.
3. Davidson CL. Glassionomer bases under posterior composites. J Esthet
Dent 1994;6:223-226.
4. De Munck J, Braem M, Wevers M, Yoshida Y, Inoue S, Suzuki K, Lam-
brechts P, Van Meerbeek B. Micro-rotary fatigue of tooth-biomaterial inter-
faces. Biomater 2005;26:1145-1153.
5. Dewji HR, Drummond JL, FadaviS, Punwani I. Bond strength of bis-GMA
and glass ionomer pit and fissure sealants using cyclic fatigue. Eur J Oral
Sci 1998;6:594-599.
6. Draughn RA. Compressive fatigue limits of composite restorative materi-
als. J Dent Res 1979;58:1093-1096.
7. Givan DA, Fitchie JG, Anderson L, Zardiackas LD. Tensile fatigue of 4-META
cement bonding three base metal alloys to enamel and comparison to
other resin cements. J Prosthet Dent 1995;73:377-385.
8. Hawbolt EB, MacEntee MI. Effects of fatigue on a soldered base metal
alloy. J Dent Res 1983;62:1226-1228.
9. Huysmans MCDNJM, Van der Varst PGT, Schäfer R, Peters MCRB, Plass-
chaert AJM, Soltész U. Fatigue behavior of direct post-and-core-restored
premolars. J Dent Res 1992;71:1145-1150.
10. McCabe JF, Carrick TE, Chadwick RG, Walls AWG. Alternative approaches
to evaluating the fatigue characteristics of materials. Dent Mater
1990;6:24-28.
11. Nakajima H, Watkins JH, Arita K, Hanaoka K, Okabe T. Mechanical proper-
ties of glass ionomers under static and dynamic loading. Dent Mater
1996;12:30-37.
12. Nikaido T, Kunzelmann K-H, Chen H, Ogata M, Harada A, Yamaguchi Y, Cox
CF, Hickel R, Tagami J. Evaluation of thermal cycling and mechanical load-
ing on bond strength of a self-etching primer system to dentin. Dent Mater
2002;18:269-275.
13. Ruse ND, Shew R, Feduik D. In vitro fatigue testing of a dental bonding sys-
tem on enamel. J Biomed Mater Res 1995;29:411-415.
14. Wiskott HWA, Nicholls JI, Belser UC. Fatigue resistance of soldered joints:
A methodological study. Dent Mater 1994;10:215-220.
Clinical relevance: Repetitive shear loading off freshly
placed adhesive fillings will impose subcritical loads
that could finally induce damage and/or loss of the ad-
hesion. The study of such behavior is therefore of ut-
most importance in order to gain knowledge on this
type of failure
253
Sarrett

254 The Journal of Adhesive Dentistry

Microleakage of Class V Composite Restorations Placed
with Etch-and-Rinse and Self-etching Adhesives Before
and After Thermocycling
Juan Ignacio Rosales-Leala

Purpose: To evaluate the sealing ability of etch-and-rinse and self-etching adhesives in Class V cavities before and
after thermocycling in vitro.

Materials and Methods: Etch-and-rinse adhesives (Prime & Bond NT [P&B], XP Bond [XPB], ScotchBond 1 XT [SBX],
Syntac [SYN]) and self-etching adhesives (Xeno III [XNO], i-Bond [IBO], Clearfil SE Bond [CLF]) were used. A microleak-
age test was performed to evaluate marginal sealing. Seventy molars were divided into seven groups according to the
adhesive used. Class V cavities were restored and each group was divided into two subgroups. One group was water
immersed for 24 h and the other was thermocycled. Then, specimens were immersed in fuchsin and sectioned. Mi-
croleakage and dentin permeability were recorded on occlusal and gingival walls and data were statistically analyzed.

Results: Etch-and-rinse adhesives provided perfect occlusal sealing. Self-etching adhesives obtained slight occlusal
leakage. In the gingival wall, XNO and CLF showed the lowest leakage, followed by XPB and SBX, then P&B. SYN and
IBO exhibited the highest leakage. All SE adhesives and XPB provided sealed dentinal tubules. Thermocycling did not
affect the occlusal sealing but reduced the gingival sealing when P&B, SYN, XNO, CLF, and IBO were used.

Conclusion: In enamel, marginal leakage was prevented when phosphoric acid was used. Self-etching adhesives pro-
moted slight occlusal leakage. The gingival sealing was poorer than the occlusal sealing. XNO, CLF followed by XPB
obtained the best gingival sealing. Thermocycling did not affect the occlusal bonding but reduced the gingival sealing,
except when XPB and SBX were used.

Keywords: adhesives, Class V sealing, thermocycling, in vitro.

J Adhes Dent 2007; 9: 255-259. Submitted for publication: 15.12.06; accepted for publication: 3.1.07.

S ealing of a cavity is one of the most important require-

ments for the durability of a composite restoration.13 Mi-
croleakage of a restoration may be the starting point of sec-
ondary caries and the treatment failure.11 The bond needs
to be hermetic but also durable over time.3,21
In vitro microleakage tests offer very useful data about
the sealing behavior of adhesives. A microleakage test pro-
vides information about the sealing of the interface and the
dentin tubule sealing (dentin permeability).1,16 Results are
close to clinical reality because extracted human teeth and
clinical protocols are used.7,11
Two different classes of adhesives are currently used.
Etch-and-rinse adhesives require a separate acid-etching
step prior to the adhesive infiltration that promotes an ag-
gressive substrate treatment.15 Self-etching adhesives etch
and infiltrate at the same time, but their acidity is less than
that of phosphoric acid, resulting in less etching depth.19
More information is necessary about the sealing ability of
current adhesives (etch-and-rinse vs self-etching) and the ef-
fect of aging on the durability of the sealing. The purpose of
this work was to evaluate the in vitro sealing ability of etch-
and-rinse and self-etching adhesives in Class V cavities be-
fore and after thermocycling.

a Assistant Professor, Department of Stomatology (Dental Materials), University

of Granada, Granada, Spain.
Paper presented at Satellite Symposium on Dental Adhesives, Dublin,
September 13th, 2006.
Reprint requests: Dr. Juan Ignacio Rosales-Leal, Camino de Ronda, 57-2ºB,
18004 Granada, Spain. Tel: + 34-653-32-03-84, Fax: +34-958-240-908.
e-mail: irosales@ugr.es
MATERIALS AND METHODS
The adhesives used are described in Table 1. Seventy third
molars were divided into 7 groups as a function of the ad-
hesive used (Table 1). In each specimen, two Class V Cavi-
ties (3 x 2 x 2 mm [depth] with a 1-mm 45-degree enamel

Vol 9, Supplement 2, 2007 255

Rosales-Leal

Table 1 Materials tested

Adhesive Manufacturer Components Directions for use

Prime & Bond NT Dentsply DeTrey; Conditioner: DeTrey Conditioner (36% Etch the cavity for 15 s, wash and dry but do
lot: 0503000835 Konstanz, Germany phosphoric acid) not desiccate. Apply the adhesive and wait
(P&B) Adhesive: (resin, di- and tri- for 20 s. Dry and polymerize for 10 s. Apply
methacrylate, amorphous functional, composite and polymerize for 20 s.
silica, PENTA, cetyl amine
hydrofluoride, acetone, photoinitiators,
stabilizers)
Composite: Esthet·X (microhybrid)

XP Bond Dentsply, DeTrey; Conditioner: DeTrey Conditioner (36% Etch the cavity for 15 s, wash and dry but do
lot: 0503004020 Konstanz, Germany phosphoric acid) not desiccate. Apply adhesive and wait for
(XPB) Adhesive: tertiary butanol, HEMA, 20 s. Dry and polymerize for 10 s. Apply
PENTA, TCB, UDMA, TEG-DMA; composite and polymerize for 20 s.
butylated benzenediol, ethyl-4-
dimethylaminobenzoate, camphoro-
quinone, nanofillers
Composite: Ceram·X mono (nano
ceramic)

Adper ScotchBond 1 XT 3M; St Paul, MN, USA Conditioner: etchant (37% phosphoric Etch cavity for 15 s, wash and dry (do not
lot: 177215 acid) desiccate). Apply adhesive and wait for 15 s.
(SBX) Adhesive: HEMA Air dry and light cure for 10 s. Place compos-
Composite: Filtek Supreme (nano ite and light cure for 20 s.
composite)

Syntac Ivoclar Vivadent; Conditioner: Total Etch (37% Etch cavity for 30 s, wash and dry. Apply
lot: G01297 Schaan, Liechtenstein phosphoric acid). primer, wait for 15 s. Air dry. Apply adhesive
[primer], G04548 Primer: polyethylene glycol dimethacry- and wait 10 s. Air dry. Apply bonding and air
[adhesive], late, maleic acid, ketone, water dry. Light cure for 10 s Place composite and
G03430 [bonding] Adhesive: polyethylene glycol light cure for 20 s.
(SYN) dimethacrylate, glutaraldehyde, water
Bonding: bis-GMA, TEG-MA
Composite: Tretic Evo Ceram
(microhybrid)

Xeno III Dentsply, DeTrey; Adhesive: A liquid (HEMA, water, Mix liquid A and B. Apply in the cavity and
lot: 0403001320 Konstanz, Germany ethanol, BHT, highly dispersed silicon wait for 20 s. Dry and polymerize for 10 s.
[A liquid], dioxide). B liquid (pyro-EMA, PEM-F, Apply composite and polymerize for 40 s.
0403001320 UDMA, BHT, camphoroquinone, ethyl-
[B liquid] (XNO) 4-dimethylaminobenzoate).
Composite: Ceram·X mono (nano
ceramic)

i-Bond Heraeus Kulzer; Adhesive: acetone, water, Apply a copious amount to the cavity. Apply
lot: 010082 Hanau, Germany methacrylate resins, glutaraldehyde two additional coats. Wait for 30 s. Dry and
(IBO) Composite: Venus (microhybrid) polymerize for 20 s. Apply composite and
polymerize for 20 s.

Clearfil SE Bond Kuraray; Primer: MDP, HEMA, hydrophilic Apply primer; wait for 20 s. Dry with mild air
lot: 00453A Okayama, Japan dimethacrylate, di-camphorquinone, flow. Apply bond. Air flow gently. Light cure
[primer]; 00623A N,N-diethanol-p-toluidine, water for 10 s, place composite and polymerize for
[adhesive] Bonding: MDP, bis-GMA, HEMA, 40 s.
(CLF) hydrophobic dimethacrylate, di-cam-
phoroquinone, N,N-diethanol-p-
toluidine, silanated colloidal silica
Composite: Clearfil AP X (microhybrid)

HEMA: 2-hydroxyethylmethacrylate; PENTA: dipentaerythriol penta acrylate monophosphate; TCB: carboxylic acid modified dimethacrylate; TEG-DMA: tri-
ethyleneglycol dimethacrylate; pyro-EMA: phosphoric acid modified methacrylate; PEM-F: monofluorophosphazene-modified methacrylate; MDP: 10-
methacryloyloxydecyl dihydrogen phosphate; UDMA: urethane dimethacrylate; bis-GMA: bis-phenol A diglycidyl methacrylate.

256 The Journal of Adhesive Dentistry


Fig 1 Percentage of cases with each
microlekage grade on the occlusal wall
(O) and on the gingival wall (G) after
24-h water immersion (24 h) and
4000 cycles of thermocycling (4000
c). Columns with the same letter are
statistically similar (p > 0.05).
bevel) were prepared with diamond-coated #330 burs at
high speed under water cooling. Cavities were filled follow-
ing manufacturer’s directions for use. The filling material
was placed in two increments. The LED unit SmartLite PS
(Dentsply DeTrey; Konstanz, Germany) (light output: 830
mW/cm2) was used for polymerization. The restoration was
finished and polished with abrasive disks. Restored teeth
were divided into two subgroups. In one group, teeth were
kept in water at 37°C for 24 h. In the other group, teeth were
thermocycled 4000 times between water baths at 5°C and
55°C with a dwell time in each bath of 30 s. After sealing the
roots with IRM (Dentsply DeTrey), the teeth were covered with
two coats of nail varnish, leaving a 1-mm varnish-free mar-
gin around the restoration. Specimens were then immersed
in a 0.5% water solution of basic fuchsin for 24 h and rinsed
for 5 min with water. After this, specimens were embedded
in acrylic resin, and 3 buccolingual slices of 1 mm thickness
were obtained from each specimen (15 slices resulting in 30
margins in dentin and enamel, per adhesive and aging con-
dition). Slices were coded and randomly examined inde-
pendently under the microscope in a blinded fashion. The
grade of microleakage at occlusal and gingival walls was cat-
egorized as follows: 0: hermetic seal, no leakage; 1: mild mi-
croleakage, dye on no more than half of the wall; 2: moder-
ate microleakage, dye on more than half of the wall but not
including the axial wall; 3: massive microleakage, dye on the
entire wall, including the axial wall. Data obtained represent
the percentage of each leakage score in all the analyzed
slices. Dentin permeability was evaluated as negative (ab-
sence of dye solution in dentin tissue) or positive (presence
of dye solution in dentin tissue). Microleakage analysis was
performed with the nonparametric Kruskal-Wallis H-test and
Vol 9, Supplement 2, 2007
Rosales-Leal
Mann-Whitney U-test (p < 0.05). Fisher’s Exact test was used
to evaluate dentin permeability (p < 0.05).
RESULTS
Figures 1 and 2 show the microleakage and dentin perme-
ability data. The occlusal wall exhibited less leakage than the
gingival wall. Etch-and-rinse adhesives achieved hermetic
occlusal sealing, while self-etching adhesives showed slight
occlusal leakage. Occlusal dentin permeability was negative
for all the adhesives tested. Thermocycling did not affect the
occlusal sealing.
On the gingival wall, XNO and CLF obtained the lowest
leakage, followed by XPB, SBX, and P&B, while SYN and IBO
showed the highest leakage. Thermocycling did not affect
marginal seal in dentin for XPB and SBX, with the latter
showing more leakage after thermocycling compared to
XPB. However, marginal seal of P&B, SYN, XNO, IBO, and CLF
was influenced by thermocycling. Dentin permeability was
negative for XPB, XNO, IBO and CLF. Positive dentin perme-
ability was observed when P&B, SBX or SYN were used. Ther-
mocycling increased the dentin positive permeability of P&B
and SYN groups.
DISCUSSION
This in-vitro test provoked microleakage for all adhesives
used. Three main factors could affect the sealing. One fac-
tor is the composite polymerization shrinkage that induces
stress at the bonding interface.8 This stress can potentially
257
Rosales-Leal
break the bond and facilitate leakage.13,19 Another factor is
that the substrate is a biological tissue, which makes adhe-
sion difficult.15 The third factor is the adhesive itself: the
chemical composition plays an important role in achieving a
strong, durable, and biologically compatible bond.11
Etch-and-rinse adhesives obtained hermetic sealing on
the occlusal wall, which is surrounded by enamel. Enamel is
mainly composed of minerals with no significant amount of
organic compounds or water.15 Use of phosphoric acid leads
to pronounced etching depth. The adhesive covers a highly
irregular mineral surface with no water, creating a hermetic
and strong bond.2,6,9,10,13 In contrast, self-etching adhe-
sives exhibited slight leakage. In general, the pH of acidic
primers is higher than that of phosphoric acid, resulting in a
less pronounced etching effect.4,21 The consequence in this
in vitro study was a weaker bond with slight leakage.6,8,15
In agreement with other studies,6,8,10,13,14 sealing was
better along occlusal than gingival margins. The gingival wall
is formed by dentin, which consists of minerals, organic
compounds (mainly collagen fibers), and water.15 In addi-
tion, dentin tubules cross the tissue and are full of water. Af-
ter phosphoric acid treatment, there is a deep demineral-
ization front in which the collagen network is exposed, dentin
tubules are opened, and water content is increased.17 Etch-
and-rinse primers have to infiltrate the exposed collagen, re-
place the water, and seal the tubules. Therefore, sealing is
complicated, and this histological finding explains the high-
er leakage and positive permeability when etch-and-rinse ad-
hesives are used. XPB was the best etch-and-rinse adhesive
in this study, and always sealed the dentin tubules. This ad-
hesive uses tertiary butanol as a solvent and provides an in-
crease in resin content. After polymerization, the bonding
258
Fig 2 Percentage of cases with posi-
tive and negative permeability on the
occlusal wall (O) and on the gingival
wall (G) after 24-h water immersion
(24 h) and 4000 cycles of thermocy-
cling (4000 c). Columns with the
same letter are statistically similar (p
> 0.05).
layer will be thicker and consist of a dense polymer matrix
that promotes better sealing.
Self-etching adhesives (except IBO) obtained higher
dentin sealing capability than etch-and-rinse adhesives. To
etch and infiltrate at the same time assures proper covering
of the demineralized dentin and avoids the problem of wa-
ter, which etch-and-rinse adhesives have after phosphoric
etching.4,11 The lower primer acidity promotes less tubule
opening,14 and then tubule sealing was demonstrated to be
easier.6 The consequence is that self-etching adhesives al-
ways sealed the dentin tubules and yielded lower leakage
than etch-and-rinse adhesives. In accordance with oth-
ers,6,15 IBO allowed more leakage than other adhesives test-
ed. Despite the higher leakage, IBO sealed always the dentin
tubules.
Evaluation of the dentin permeability to the dye solution
shows the adhesive ability to seal the dentin tubules.16 With-
in the limits of a microleakage study (not being a nanoleak-
age evaluation), it can be concluded that if there is leakage
but no positive permeability, the interface failure will be lo-
cated over the intact dentin. In this situation, penetrating
bacteria will be surrounded by resin interfaces which could
slow down secondary caries development. In fact, pulp in-
flammation was measured in vivo,12 and when the bacteria
progressed between the cavity and the composite, a low lev-
el of pulp inflammation was found. However, if the bacteria
progress into the dentin tubules, the inflammatory activity is
higher.3 Therefore, it is desirable to achieve sealing of denti-
nal tubules.
Thermocycling is an easy method to age restorations and
results in the highest clinically relevant stress.3,18 As was
demonstrated in others studies,18 thermocycling did not af-
The Journal of Adhesive Dentistry

fect the occlusal sealing and showed that the enamel junc-
tion is resistant to aging, due to the mineral nature of the tis-
sue which ensures a better and more durable bond.4 In con-
trast, the dentin bond was susceptible to damage and the
sealing was reduced after thermocycling.18 The larger pro-
portion of organic compounds and water in the dentin
makes the union weaker for all the adhesives tested, which
would explain aging.11,17 Thermocycling accelerates the ag-
ing by hydrolytic degradation of the hydrophilic components
in the bonding system.12,22 In addition, repetitive contrac-
tion/expansion stress at the bonding interface may lead to
cracks that propagate along the interface and cause in- and
outflow of fluids.5 When considering distribution of mi-
croleakage grades in all obtained slices, only XPB was not
affected by thermocycling.
Clinically, when a cavity is surrounded by enamel, the
phosphoric acid will ensure a hermetic and durable bond.
When the cavity margins are in dentin, improvements are
necessary, but there are some self-etching adhesives (XNO,
CLF) or etch-and-rinse adhesives (XPB) that obtain excellent
results with no positive dentin permeability and low leakage.
Perhaps more acidic primers could improve the sealing of
composite resin restorations.
CONLUSIONS
In enamel, no microleakage was found when phosphoric
acid was used, but self-etching adhesives showed slight
leakage. The gingival sealing was inferior to the occlusal
sealing. XNO and CLF obtained the best gingival sealing, fol-
lowed by XPB, SBX, P&B, and IBO, with SYN demonstrating
the worst sealing. Self-etching adhesives and XPB were able
to hermetically seal the dentin tubules (negative permeabil-
ity). Thermocycling did not affect the occlusal bonding or XPB
gingival sealing.
ACKNOWLEDGMENTS
This research was sponsored by Dentsply DeTrey, Konstanz, Germany.
REFERENCES
1. de la Torre-Moreno FJ, Rosales-Leal JI, Bravo M. Effect of cooled composite
inserts in the sealing ability of composite resin restorations placed at intra-
oral temperatures: an in vitro study. Oper Dent 2003;28:297-302.
2. De Munck J, Van Landuyt K, Peumans M, Poitevin A, Lambrechts P, Braem
M, Van Meerbeek B. A Critical Review of the Durability of Adhesion to Tooth
Tissue: Methods and Results. J Dent Res 2005;84:118-132.
Vol 9, Supplement 2, 2007
Rosales-Leal
3. De Munck J, Vargas M, Iracki J, Van Landuyt K, Poitevin A, Lambrechts P,
Van Meerbeek B. One day bonding effectiveness of new self-etch adhe-
sives to bur-cut enamel and dentin. Oper Dent 2005;30:39-49.
4. Frankenberger R, Krämer N, Petschelt A. Long-term effect of dentin
primers on enamel bond strength and marginal adaptation. Oper Dent
2000;25:11-19.
5. Gale MS, Darvell BW. Thermal cycling procedures for laboratory testing of
dental restorations. J Dent 1999;27:89-99.
6. Gueders AM, Charpentier JF, Alber AI, Geerts SO. Microleakage after ther-
mocycling of 4 etch and rinse and 3 self-etching adhesives with and with-
out flowable composite lining. Oper Dent 2006;31:450-455.
7. Hilton TJ. Can modern procedures and materials reliably seal cavities?. In
vitro investigations. Part I. Am J Dent 2002;15:198-210.
8. Kleverlaan CJ, Feilzer AJ. Polymerization shrinkage and contraction stress
of dental composites. Dent Mater 2005;21:1150-1157.
9. Koliniotou-Koumpia E, Dionysiopoulos P, Koumpia E. In vivo evaluation of
microleakage from composites with new dentin adhesives. J Oral Rehabil
2004;31:1014-1022.
10. Manhart J, Chen HY, Mehl A, Weber K, Hickel R. Marginal quality and mi-
croleakage of adhesive class V restorations. J Dent 2001;29:123-130.
11. Mjör IA, Shen C, Eliasson ST, Richter S. Placement and replacement of
restorations in general dental practice in Iceland. Oper Dent 2002;
27:117–123.
12. Murray PE, Hafez AA, Smith AJ, Cox CF. Bacterial microleakage and pulp in-
flammation associated with various restorative materials. Dent Mater
2002;18:470-8.
13. Nakabayashi N, Pashley DH. Hybridization of dental hard tissues. Tokio:
Quintessence 1998.
14. Oliveira SSA, Marshall SJ, Hilton JF, Marshall GW. Etching kinetics of a self-
etching primer. Biomaterials 2002;23:4105-4112.
15. Owens BM, Johnson WW. Effecto of insertion technique and adhesive sys-
tem on microleakage of Class V resin composite restorations. J Adhes Dent
2005;7:303-308.
16. Rosales-Leal JI, de la Torre-Moreno FJ, Bravo M. Effect of pulp pressure on
the micropermeability and sealing ability of etch&rinse and self-etching ad-
hesives. Oper Dent 2006; in press.
17. Salz U, Zimmermman J, Zeuner F, Moszner N. Hydrolitic stability of self-
etching adhesive systems. J Adhes Dent 2005;7:107-116.
18. Schuckar M, Geurtsen W. Proximo-cervical adaptation of class II-compoite
restorations after thermocycling: a quantitative and qualitative study. J
Oral Rehabil 1997;24:766-775.
19. Tay FH, Pashley DH. Aggressiveness of contemporary self-etching systems:
I: Depth of penetration beyond dentin smear layers. Dent Mater 2001;
17:296-308.
20. Van Meerbeek B, InokoshiS, Braem M, Lambrechts P, Vanherle G. Morpho-
logical aspects of the resin-dentin interdiffusion zone with different dentin
adhesive systems. J Dent Res 1992;71:1530-1540.
21. Van Meerbeek B, Perdigão J, Lambrechts P, Vanherle G. The clinical perfor-
mance of adhesives. J Dent 1998;26:1-20.
22. Yang B, Adlung R, Ludwig K, Böbmann K, Pashley DH, Kern M. Effect of
structural change of collagen fibrils on the durability of dentin boning. Bio-
materials 2005;26:5021-5031.
Clinical relevance: Phosphoric acid ensures hermetic
and durable union on enamel. Although there are some
excellent adhesives, it is nesessary to improve the
dentin sealing.
259
Sarrett

260 The Journal of Adhesive Dentistry

Microleakage of XP Bond in Class II Cavities After
Artificial Aging
Jürgen Manharta/Cordula Trummb

Purpose: To determine the microleakage of etch and rinse adhesives.

Materials and Methods: Standardized Class II cavities were cut in 40 human molars with one proximal box limited
within enamel and one proximal box extending into dentin. Teeth were assigned randomly to 5 groups (n = 8) and re-
stored with incrementally placed composite restorations. Five combinations were tested: G1 = XP Bond + CeramX
Mono, G2 = Syntac Classic + Tetric EvoCeram, G3 = Scotchbond 1 XT + Z250, G4 = P&B NT + CeramX Mono, G5 =
Optibond Solo Plus + CeramX Mono. After finishing and polishing, teeth were stored for 48 h in water at 37°C before
being subjected to artificial aging by thermal stress (5/55°C, 2000x, 30 s) and mechanical loading (50 N, 50,000x).
Teeth were isolated with nail varnish and immersed in 5% methylene blue for 1 h. After sectioning, specimens were
evaluated for leakage (ordinal scale: 0 to 4) at enamel and dentin margins under a stereomicroscope. Results were
analyzed using the Kruskal-Wallis H-test and Mann-Whitney U-test (p < 0.05).

Results: Statistical analysis showed significant differences among the groups in both enamel and dentin. Mean
ranks (H-test) were: enamel: G2 (64.44) < G1 (66.69) < G4 (74.88) < G3 (98.25) and G5 (98.25); dentin: G3 (65.53) <
G1 (74.42) < G4 (81.09) < G2 (81.84) < G5 (99.61).

Conclusion: Microleakage of XP Bond is at the same level as or even better than other etch-and-rinse adhesives.

Keywords: Class II restorations, dentin adhesives, composite, microleakage.

J Adhes Dent 2007; 9: 261-264. Submitted for publication: 15.12.06; accepted for publication: 8.1.07.

D espite improvements in the formulation of modern

dentin adhesive systems, the bond strength and mar-
ginal adaptation of composite resins to dentin seems still in-
ferior and less predictable than adhesion to enamel.3,11
However, most of the cavities in clinical dentistry, especially
when restorations in the posterior region of the mouth are
replaced, are not limited exclusively within enamel but show
a mixed type configuration with finishing lines in both enam-
el and dentin.3,12 In particular, the adhesive interface be-
tween tooth and restorative material at the gingival finish
line has been recognized as one of the most problematic re-
gions.5,9 While a great number of self-etching primers and
adhesives have emerged on the market, which are consid-
ered less technique sensitive and less time consuming than
etch-and-rinse adhesives,13 the latter are still considered
the gold standard with respect to long-term bond strength
and marginal seal, especially for the restoration of highly
loaded Class II cavities or when restorations are bonded to
uninstrumented tooth tissues such as sclerotic dentin in
Class V lesions or virgin enamel in anterior diastema clo-
sures.
This study assesses the microleakage of a newly formu-
lated etch-and-rinse adhesive, based on a tert-butanol sol-
vent used for the first time, in large Class II cavities after ar-
tificial aging in comparison with well-established competitive
adhesive and composite systems. The null hypothesis test-
ed was that the type of restorative system used does not sig-
nificantly affect the marginal seal.

a Associate Professor, Department of Restorative Dentistry, Ludwig Maximil-

ians University, Munich, Germany. MATERIALS AND METHODS
b Dentist in Private Practice, Munich, Germany.

Paper presented at Satellite Symposium on Dental Adhesives, Dublin, Specimen Preparation

September 13th, 2006.
Reprint requests: Dr. Jürgen Manhart, Department of Restorative Dentistry,
Goethe Street 70, 80336 Munich, Germany. Tel: +49-89-5160-7610, Fax: +49-
89-5160-9302. e-mail: manhart@manhart.com
Forty freshly extracted caries-free human permanent mo-
lars, stored in a 0.25% mixture of sodium azide in Ringer so-
lution until the date of use, were used in this in vitro study.
After cleaning the teeth with scalers and polishing with

Vol 9, Supplement 2, 2007 261

Manhart/Trumm
Table 1 Experimental groups and materials used
Group Adhesive
G1 XP Bond (Dentsply
DeTrey; Konstanz, Germany
G2 Syntac Classic
(Ivoclar Vivadent;
Schaan, Lichtenstein
G3 Scotchbond 1 XT
(3M ESPE; Seefeld, Germany)
G4 Prime & Bond NT (Dentsply
DeTrey; Konstanz, Germany
G5 Optibond Solo Plus (Kerr-Hawe;
Bioggio, Switzerland
pumice, standardized Class II inlay cavities (MOD) were pre-
pared, with one proximal box limited within enamel (1 to 1.5
mm above the cementoenamel junction) and one proximal
box extending into dentin (1 to 1.5 mm below the cemen-
toenamel junction) (Fig 1). The cavities were 4.0 mm in width
and 3 to 3.5 mm in depth at the occlusal isthmus and 5.0
mm in width at the proximal boxes. The depth of the proxi-
mal boxes in the direction of the axial pulpal walls was 1.5
mm. To achieve divergence angles between opposing walls
of 10 to 12 degrees, cavities were prepared using coarse di-
amond burs with a slight taper (855.314, Komet; Lemgo,
Germany) in a high-speed dental handpiece with copious wa-
ter spray. Fine grained diamond burs of the same shape
(8855.314, Komet) were used for finishing the preparations.
The internal point and line angles were rounded and enam-
el margins were not beveled but prepared in butt-joint con-
figuration.11 After visual inspection of the cavities for im-
perfect finish lines, the 40 prepared teeth were randomly as-
signed to 5 experimental groups with 8 teeth each (Table 1),
corresponding to the different restorative techniques. Man-
ufacturers' instructions for each material were strictly fol-
lowed.
For the direct composite restorations, all enamel and
dentin surfaces of the cavities were conditioned with 36%
phosphoric acid gel (DeTrey Conditioner 36, Dentsply De-
Trey; Konstanz, Germany), starting acid application on enam-
el, leaving undisturbed for 15 s, then covering the dentinal
preparation surfaces for an additional 15 s (total-etch tech-
nique). After thoroughly rinsing with water, the cavities were
then gently dried with oil-free compressed air, taking care to
avoid desiccation of the tooth substrate (moist bonding tech-
nique). Following the application and light curing of the ad-
hesive systems, the cavities were restored with composite
resin (Table 1) using a horizontal and oblique layering tech-
nique with 5 increments in the dentin-limited proximal box
and 4 increments in the enamel-limited box (Fig 1). Each in-
crement with a maximum thickness of 2 mm was light cured
individually with a LED curing unit (SmartLite PS, Dentsply
DeTrey) according to the manufacturer’s recommendations.
The light output of the curing unit was monitored at 1065
262
Solvent type of Composite
adhesive
t-butanol Ceram-X Mono (M2)
(Dentsply DeTrey)
Primer: acetone-water Tetric EvoCeram (A2)
Adhesive: water (Ivoclar Vivadent)
Heliobond: -
Ethanol-water Z250 (A2)
(3M ESPE)
Acetone Ceram-X Mono (M2)
(Dentsply DeTrey)
Ethanol Ceram-X Mono (M2)
mW/cm2 with a calibrated light meter (CureRite, Dentsply
DeTrey). All restorations were finished and polished imme-
diately after placement using finishing diamond burs and
polishing disks (Sof-Lex, 3M ESPE; Seefeld, Germany).
Thermocycling and Mechanical Loading
After 48 h storage in distilled water at 37°C, the restored
teeth were subjected to artificial aging by thermocycling and
mechanical loading. All specimens were immersed alter-
nately in water baths at 5°C and 55°C for 2000 cycles, with
a dwell time of 30 s in each bath and a transfer time of 15
s. Mechanical loading of the teeth, which were mounted on
metallic specimen holders with a light-curing composite, was
conducted in the Munich Oral Environment.8 The carefully
aligned teeth were loaded in the central fossa of the restora-
tions in axial direction with a force of 50 N for 50,000 times
at a frequency of 1 Hz. The antagonist material was a De-
gusit sphere 6 mm in diameter, which exhibits a hardness
and wear resistance similar to natural enamel.8,19-21 The
metal specimen holders were mounted on a hard rubber el-
ement, which allowed a sliding movement of the tooth be-
tween the first contact on an inclined plane to the central
fossa.4 During mechanical loading, the teeth were continu-
ously immersed in Ringer solution. This oral simulation de-
vice exhibits similar functions to the machine developed by
Krejci.7
Evaluation of Microleakage
The apices of the artificially aged teeth were sealed with ad-
hesive and composite (Prime & Bond NT and Ceram-X
Mono). All tooth surfaces were covered with 2 coats of nail
varnish to within approximately 1 mm of the margin of the
restoration. Microleakage was tested using a standardized
dye penetration method. The specimens were immersed in
5% methylene blue at 37°C for 1 hour and then rinsed with
tap water. Teeth were embedded in clear acrylic auto-poly-
merizing resin (Technovit, Kulzer; Wehrheim, Germany). All
restorations were sectioned longitudinally with two parallel
cuts in three fragments in mesiodistal direction with a wa-
ter-cooled low-speed diamond saw (Varicut, Leco; Kirch-
The Journal of Adhesive Dentistry
 Manhart/Trumm

heim, Germany), resulting in four readings for each speci-

men at the enamel and dentin adhesive interface. An ordi-
nal scale from 0 to 4 was used to score microleakage sep-
arately at the enamel and dentin margins of each section
(Fig 2).6 Each section was examined under a stereomicro-
scope (Stemi SV 11, Zeiss; Oberkochen Germany) at 40X
magnification and scored by two examiners. Consensus was
forced if disagreements occurred.16 The results of the mi-
croleakage investigation were analyzed using the nonpara-
metric Kruskal-Wallis H-test and post-hoc Mann-Whitney
U-test at a significance level of p < 0.05.

RESULTS

Microleakage results are presented in Table 2. The Kruskal-

Wallis H-test revealed statistically significant differences
among the experimental groups in the enamel (p = 0.001)
and dentin margins (p = 0.022) of the Class II restorations.

DISCUSSION
Microleakage studies provide adequate screening methods,
possibly determining what kind of adhesive system will show
acceptable clinical performance.13 While quantitative mar-
ginal analysis by scanning electron microscopy assesses the
entire circumference of the tooth/restoration interface, it can
only determine the quality of the adhesive interface at the
cavosurface margin. The extension of marginal gaps towards Fig 1 Incremental restoration technique and light curing direc-
the axial wall of restorations is commonly assessed by mi- tion.11
croleakage studies.10 Detection of microleakage can be ac-
complished with a number of techniques, including bacteria,
chemical or radioactive tracer molecules, fluid permeability, hand, water-based systems are not as sensitive with regard
and dye penetration.1 The most common technique is the to dentin moisture content, as they have inherent rewetting
use of dyes, the penetration of which is determined after sec- properties, but require a longer evaporation time for the sol-
tioning of the specimen with a magnifying aid. vent, because water has a considerably lower vapor pres-
The type of solvent strongly influences the clinical appli- sure than acetone.18 If the solvent is not completely evapo-
cation protocol of etch-and-rinse adhesive systems. Acetone- rated before light curing the adhesive, flaws can weaken the
based systems only work well on a moist dentin surface as hybrid layer, probably causing premature restoration failure.2
acetone is a water chaser and can lead to rather poor results A new type of solvent for adhesives, namely, tert-butanol, was
on overdried acid-etched dentin surfaces. On the other introduced for XP Bond. Tert-butanol (2-methyl-2-propanol)

Table 2 Microleakage frequency scores at enamel and dentin margins in the experimental groups G1 to G5.

Enamel Dentin
Leakage 0 1 2 3 4 Mean rank Leakage 0 1 2 3 4 Mean rank
score (Kruskal- score (Kruskal-
Wallis) Wallis)
G1 28 0 4 0 0 66.69a G1 20 3 4 5 0 74.4A
G2 28 3 1 0 0 64.44a G2 18 1 7 4 2 81.84A,B
G3 15 7 9 1 0 98.25b G3 23 5 1 2 1 65.53A
G4 24 4 4 0 0 74.88a G4 19 2 2 7 2 81.09A,B
G5 15 7 9 1 0 98.25b G5 10 6 7 6 3 99.61B

Different superscript letters indicate statistically significantly different subsets within each margin segment as determined by post-hoc
multiple comparisons with the Mann-Whitney U-test (p < 0.05)

Vol 9, Supplement 2, 2007 263

Manhart/Trumm
consists of a C4 body with an alcohol group surrounded by 3
methyl groups, making it totally miscible both with water and
polymerizable resins. Although tert-butanol has a higher mol-
ecular weight than ethanol, the evaporation rate is almost the
same, with a latent heat of vaporization of 41 kJ/mol for tert-
butanol and 42 kJ/mol for ethanol.15 Vapor pressure of the
different kinds of solvents at 20°C is given as 2330 Pa for wa-
ter, 4133 Pa for tert-butanol, 5900 Pa for ethanol, and
23,300 Pa for acetone.14 The properties of tert-butanol make
it possible to use a dappen dish and increase the resin con-
tent of the adhesive, which results in an increase of adhesive
layer thickness and a higher degree of technique robustness
as compared to acetone-based systems. The solvent used for
etch-and-rinse adhesives is a major factor affecting handling
characteristics and performance.2,17
CONCLUSIONS
The two-step one-bottle tert-butanol-based XP Bond showed
excellent microleakage results in both enamel and dentin,
with the same quality as a well-established three-step etch-
and-rinse system.
ACKNOWLEDGEMENTS
This research was sponsored by Dentsply DeTrey, Konstanz, Germany
. 19. Wassell RW, McCabe JF, Walls AWG. Subsurface deformation associated
REFERENCES
1. Alani AH, Toh CG. Detection of microleakage around dental restorations: a
review. Oper Dent 1997;22:173-185.
2. De Munck J, Van Landuyt K, Peumans M, Poitevin A, Lambrechts P, Braem
M, Van Meerbeek B. A critical review of the durability of adhesion to tooth
tissue: methods and results. J Dent Res 2005;84:118-132.
3. Dietrich T, Lösche AC, Lösche GM, Roulet JF. Marginal adaptation of direct
composite and sandwich restorations in Class II cavities with cervical mar-
gins in dentine. J Dent 1999;27:119-128.
4. Dietschi D, Herzfeld D. In vitro evaluation of marginal and internal adapta-
tion of class II resin composite restorations after thermal and occlusal
stressing. Eur J Oral Sci 1998;106:1033-1042.
264
Fig 2 Scoring system for microleakage
evaluation in enamel and dentin.
5. Dietschi D, Scampa U, Campanile G, Holz J. Marginal adaptation and seal
of direct and indirect class II composite resin restorations: An in vitro eval-
uation. Quintessence Int 1995;26:127-138.
6. Hilton TJ, Ferracane JL. Cavity preparation factors and microleakage of
class II composite restorations filled at intraoral temperatures. Am J Dent
1999;12:123-130.
7. Krejci I, Reich T, Lutz F, Albertoni M. In-vitro-Testverfahren zur Evaluation
dentaler Restaurationssysteme. 1. Computergesteuerter Kausimulator.
Schweiz Monatsschr Zahnmed 1990;100:953-960.
8. Kunzelmann KH. Verschleissanalyse und -quantifizierung von Füllungsma-
terialien in vivo und in vitro. Aachen: Shaker-Verlag 1998.
9. Lutz F, Kull M. The development of a posterior tooth composite system, in-
vitro investigation. Schweiz Monatsschr Zahnmed 1980;90:455-483.
10. Manhart J, Chen HY, Mehl A, Weber K, Hickel R. Marginal quality and mi-
croleakage of adhesive class V restorations. J Dent 2001;29:123-130.
11. Manhart J, Hollwich B, Mehl A, Kunzelmann KH, Hickel R. Randqualität von
Ormocer- und Kompositfüllungen in Klasse-II-Kavitäten nach künstlicher Al-
terung. Dtsch Zahnärztl Z 1999;54:89-95.
12. Mayer R. Ästhetisch-adhäsive Füllungstherapie im Seitenzahngebiet - eine
Illusion? Dtsch Zahnärztl Z 1991;46:468-470.
13. Owens BM, Johnson WW, Harris EF. Marginal permeability of self-etch and
total-etch adhesive systems. Oper Dent 2006;31:60-67.
14. Roempps Chemie-Lexikon. 8th Edition, Stuttgart: Franckh-Fachlexikon
1981.
15. Scientific Compendium: XP Bond universal total-etch adhesive. Konstanz:
DENTSPLY DeTrey 2006.
16. Swift EJ, Triolo PT, Barkmeier WW, Bird JL, Bounds SJ. Effect of low-viscos-
ity resins on the performance of dental adhesives. Am J Dent 1996;9:100-
104.
17. Tay FR, Gwinnett AJ, Wei SHY. Relation between water content in acetone /
alcohol based primer and interfacial ultrastructure. J Dent 1998;26:147-
156.
18. Van Meerbeek B, De Munck J, Yoshida Y, Inoue S, Vargas M, Vijay P, Van
Landuyt K, Lambrechts P, Vanherle G. Adhesion to enamel and dentin: Cur-
rent status and future challenges. Oper Dent 2003;28:215-235.
with hardness measurements of composites. Dent Mater 1992;8:218-
223.
20. Wassell RW, McCabe JF, Walls AWG. A two-body frictional wear test. J Dent
Res 1994;73:1546-1553.
21. Wassell RW, McCabe JF, Walls AWG. Wear characteristics in a two-body
wear test. Dent Mater 1994;10:269-274.
Clinical relevance: The new tert- butanol- based XP
Bond is expected to show good clinical results due to its
chemical composition and technique robustness.
The Journal of Adhesive Dentistry
Six-month Clinical Evaluation of XP BOND in Noncarious
Cervical Lesions
Uwe Bluncka/Katharina Knitterb/Klaus-Roland Jahnc

Purpose: To evaluate the 6-month clinical performance of the etch-and-rinse one-bottle adhesive system XP BOND,
used in combination with the composite resin CeramX Duo for the restoration of Class V noncarious cervical lesions
(NCCL).

Materials and Methods: XP BOND was tested in a total of 40 patients who received two Class V CeramX Duo restora-
tions, Adper Scotchbond 1 XT was used as a control. After cleaning the teeth, the surface of the NCCL was treated
using a carbide bur in dentin and a 40-μm diamond bur in enamel with no retentive preparations. The lesions were
filled with two increments of CeramX Duo after the application of the respective adhesive by a single operator accord-
ing to manufacturer’s instructions. After 6 months, the retention and the marginal integrity were evaluated.

Results: Thirty-eight of 40 patients were evaluated after 6 months by two clinicians according to modified USPHS cri-
teria, and all restorations using XP BOND were still in place. In the control group (using Adper Scotchbond 1XT), one
restoration was lost. The statistical evaluation (chi2 test) showed no significant differences in any of the criteria. No
difference of marginal integrity was found between the two adhesive systems.

Conclusion: XP BOND meets the ADA success criteria after 6 months.

Keywords: clinical study, noncarious cervical lesions, Class V restorations, adhesive systems.

J Adhes Dent 2007; 9:265-268. Submitted for publication: 15.12.06x; accepted for publication: 3.1.07.

I n operative dentistry, etch-and-rinse systems form an im-

portant group of bonding agents that are clinically widely
used. However, as these systems require the demineraliza-
tion of dentin and the exposure of the embedded collagen
network, numerous concerns regarding drying of the protein
mesh arise.5,6,8 This is due to the need to rinse and carefully
a Associate Professor, Charité-Universitätsmedizin Berlin, Dental School, Cam-
pus Virchow Clinic, Berlin, Germany.
b Assistant Professor, Charité-Universitätsmedizin Berlin, Dental School, Cam-
pus Virchow Clinic, Berlin, Germany.
c Professor, Charité-Universitätsmedizin Berlin, Dental School, Campus Virchow
Clinic, Berlin, Germany.
Paper presented at Satellite Symposium on Dental Adhesives, Dublin,
September 13th, 2006.
Reprint requests: Dr. Uwe Blunck, Charité-Universitätsmedizin Berlin, Dental
School, Campus Virchow Clinic, Augustenburger Platz 1, 13353 Berlin, Ger-
many. Tel: +49-30-450-562-673, Fax: +49-30-450-562-961. e-mail:
uwe.blunck@charite.de
dry the surface after acid etching, in order to enable the con-
stituents of the bonding system, specifically the uncured
monomers, to penetrate the outer layers of the prepared
dentin. It has therefore been proposed that a bonding sys-
tem capable of penetrating dry and collapsed demineralized
dentin would improve bonding, resulting in better clinical
performance.8
XP BOND is a new one-bottle etch-and-rinse adhesive,
composed of a pre-mixed solution of monomers dissolved in
tert-butanol. Due to an improved ability to diffuse through
partially collapsed demineralized dentin, it is claimed to be
less technique sensitive.2
As for any other new dental restorative, data from clinical
investigations are crucial to assess the effectiveness and re-
liability of the product before being launched. This is need-
ed in order to validate results from the in vitro studies. As
generally accepted for investigating the clinical effective-
ness of such adhesive systems, noncarious Class V restora-
tions are the standard test.9,13 This is due to the fact that
they do not provide any macromechanical retention, they re-
quire at least 50% bonding to dentin, and they are widely

Vol 9, Supplement 2, 2007 265

Blunck et al
Table 1 Materials used in the study
Material Manufacturer Batch No/expiration date
XP BOND Dentsply 0512004001/2006-07
(K-0127.04)
Adper 3M ESPE 214747/2007-04
Scotchbond
1 XT
Ceram•X Duo Dentsply D1: 0119
D2: 1617
D3: 0174
D4: 0116 2008-03
DB: 1381
E1: 0583
E2: 2507
E3: 2624
available, usually found in anterior teeth or premolars with
good access for easy restoring and evaluation.
The purpose of this investigation was to evaluate the ef-
fectiveness of XP BOND compared to Adper Scotchbond 1
XT when used to restore noncarious cervical lesions, both
materials being applied with the etch-and-rinse technique.
MATERIALS AND METHODS
In 40 patients bearing noncarious cervical lesions (NCCL),
80 Class V restorations were placed with either XP BOND or
Adper Scotchbond 1 XT (Table 1). Both agents were used ac-
cording to manufacturer’s instructions, combined with the
composite resin CeramX Duo, and completed by a single op-
erator. The patients (age range 24 to 77, 17 females and 23
males) were all treated within the framework of the student
courses of the Charité Dental School in Berlin, Campus Vir-
chow Clinic. The reasons for treatment were esthetic con-
siderations, hypersensitive cervical dentin, or prevention of
further erosion. The agreement for voluntary participation
and informed consent were obtained prior to treatment. Ap-
proval for this study was given by the Ethics Committee of the
Charité Berlin (EA2/230/05, Protocol-Nr.: 14.1165).
Each lesion was initially cleaned with a nonfluoridated
polishing paste (Pellex, KerrHawe; Bioggio, Switzerland) on
a slowly rotating rubber cup, washed, and slightly dried. The
dentin surface was treated using a carbide bur (air cooled)
and the enamel margins were trimmed with a 40-μm dia-
mond bur under water spray. Saliva control was maintained
by cotton rolls. For both adhesive systems, 36% phosphoric
acid (DeTrey Conditioner 36, Dentsply DeTrey; Konstanz,
Germany) was used for standard etching (30 s on enamel
and then 15 s on dentin). After rinsing for at least 15 s, the
cavity was carefully dried without desiccating the dentin. A
single layer of XP BOND was applied for 20 s and the solvent
was evaporated for at least 5 s until a glossy surface was
266
seen. Adper Scotchbond 1 XT was applied as recommend-
ed for 15 s in 2 or 3 layers, then carefully dried for at least 5
s, resulting in a glossy surface. Both adhesives were light
cured for 10 s (Smartlite PS, Dentsply DeTrey) before the ap-
plication of CeramX Duo in at least two increments (de-
pending on the extension of the cervical lesion); each incre-
ment was light cured for 40 s. The restorations were then fin-
ished and polished by using the PoGo (Dentsply DeTrey) pol-
ishing system.
The patients were recalled after 3 and 6 months. The
restorations were checked by two evaluators. The criteria of
interest were retention, postoperative sensitivity, marginal
discoloration, margin integrity, secondary caries, and con-
tour, using the modified USPHS criteria.1,17 A vitality test was
performed and the color match of the restoration with the
surrounding tooth structure was also evaluated by the pa-
tients.
RESULTS
As seen from the results listed in Table 2, 6 months after
placement, 38 out of 40 patients were available for recall.
All restored teeth were still in contact with their antagonists
(checked during laterotrusion) with 60% showing active wear
facettes. All restorations placed with XP BOND were still in
place and showed no marginal discoloration, while in the
control group, one restoration was lost and two (5.4%)
showed discoloration of less than 50% of the margin length.
In neither group were visible margin irregularities found, and
the margins were not detectable with a dental probe. No sec-
ondary caries and no surface staining were noted. With XP
Bond, one restored tooth showed postoperative hypersensi-
tivity after 6 months, while in the control group, two teeth
were hypersensitive.
Chi2 tests were performed using the SPSS (SPSS 12.0 for
Windows, SPSS; München, Germany) statistical package.
We found no significant differences for the different criteria
between the test XP BOND and the control adhesive.
DISCUSSION
Within the limitations of a 6-month clinical study, our data
clearly show the favorable results for XP BOND. The retention
of all restorations of the treated NCCLs and the lack of stain-
ing at the margins, combined with ease of use, show much
promise for similar and other types of restorations as well.
This study, performed in accordance with manufacturer’s in-
structions, did not attempt to test this product under ex-
treme desiccation conditions, for which it is presumed to
have an advantage.2 Rather, our work was used to assess
the clinical performance of XP BOND under “normal”, rea-
sonable clinical conditions.
This study was designed to test XP BOND under a rather
well-defined clinical challenge: the treatment of NCCLs.
Class V restorations, used to treat this type of lesion, are a
reasonable choice for a clinical evaluation of a new adhesive
system because the bonding efficacy and handling charac-
teristics are exposed to a realistic and trying intraoral situa-
The Journal of Adhesive Dentistry
 Blunck et al

Table 2 Results of the clinical assessment in% of the modified USPH criteria

Criteria for XP BOND [%] Adper Scotchbond 1XT [%]

evaluated
restorations n alpha bravo charlie delta n alpha bravo charlie delta

Retention 38 100 0 0 0 38 97.4 0 0 2.6

Postoperative 38 97.4 2.6 0 0 37 94.6 5.4 0 0

sensitivity (∑)

Marginal 38 100 0 0 0 37 94.6 5.4 0 0

discoloration

Marginal 38 100 0 0 0 37 100 0 0 0

integrity

Secondary 38 100 0 0 0 37 100 0 0 0

caries

Restoration 38 100 0 0 0 37 100 0 0 0

contour

Vitality test 38 100 0 0 0 37 100 0 0 0

tion. A variety of factors, such as the nutrition of the patient,
parafunction, chewing habits, oral hygiene etc, modify the
dentin surface such that the morphology and microstructure
are different compared to surfaces that are exposed during
cavity preparation.12 Thus, tubules of cervical dentin are ex-
posed to the oral environment for a longer period and are fre-
quently partially or totally occluded with precipitates. This
forms a hypermineralized dentin layer that has been found
to be more resistant to etching.4,10 As a result, a thinner hy-
brid layer is formed on the surface, which is different from
the situation in noncervical, cut dentin.12 It has been shown
that the etch-and-rinse technique results in higher bond
strengths than self-etching adhesive systems.11 However,
etching dentin with phosphoric acid involves a sensitive
step, namely, the careful drying of the exposed collagen net-
work.5 This network has to be penetrated completely when
the adhesive system is applied. The results of this study sug-
gest that XP BOND can produce an effective bond, which is
reflected by the lack of discoloration and the retention re-
sults, as judged by two experienced dentists who have con-
siderable experience with similar, previous clinical studies.
An additional advantage of the use of a model based on
the treatment of NCCLs is that Class V restorations minimize
the influence of the operator variability. They also simplify
the evaluation procedure of margin integrity, owing to the di-
rect accessibility during the study period.9,13 We note, how-
ever, that the margins of Class V restorations cover both
enamel and dentin, and this might increase the retention
due to bonding to the acid-etched enamel. Consequently,
failure might develop due to reduced adhesion to dentin,
which is less suited to withstand mechanical stress during
mastication. Our evaluation of marginal staining and prob-
ing as well as the evaluation of hypersensitivity was aimed
at identifying failures of this type; none were found.
This evaluation is one part of a multicenter study. At pre-
sent, the results after 6 months of an identical in vivo study
at the University of Bologna, with 30 patients are available.
The criteria retention, marginal discoloration, margin in-
tegrity, secondary caries, and restoration contour (Table 3)
were all highly rated (alpha USPHS rating) for restorations in
the XP BOND group, where only one restoration (3.3%) ex-
hibited postoperative sensitivity. In the group using Adper
Scotchbond 1 XT, all criteria received a 100% alpha rating,
with postoperative sensitivity occurring in 7 teeth (23.3%)
with a bravo USPHS rating.
CONCLUSION
It should be borne in mind that these results are preliminary.
Further studies, which are to include other cavity designs
and longer observation periods, can only help to establish
the long-term reliability and the effect on the margin integri-
ty of the oral environment. However, from the present study,
it can be concluded that the results for the one-bottle etch-
and-rinse adhesive system XP BOND meet the criteria for a
provisional acceptance according to ADA guidelines, with
less than 5% failure rate after 6 months of clinical perfor-
mance.
ACKNOWLEDGMENTS
This study was funded by Dentsply DeTrey, Konstanz, Germany.

Vol 9, Supplement 2, 2007 267

Blunck et al

Table 3 Reference data obtained from the clinical assessment in % of the modified USPH criteria from the study center,
Bologna

Criteria for XP BOND [%] Adper Scotchbond 1XT [%]

evaluated
restorations n alpha bravo charlie delta n alpha bravo charlie delta

Retention 30 100 0 0 0 30 100 0 0 0

Postoperative
sensitivity (∑) 30 96.7 3.3 0 0 30 76.7 23.3 0 0

Marginal 30 100 0 0 0 30 100 0 0 0

discoloration

Marginal 30 100 0 0 0 30 100 0 0 0

integrity

Secondary 30 100 0 0 0 30 100 0 0 0

caries

Restoration 30 100 0 0 0 30 100 0 0 0

contour

Vitality test 30 100 0 0 0 30 100 0 0 0

REFERENCES
1. Barnes DM, Blank LW, Gingell JC, Gilner PP. A clinical evaluation of a resin-
modified glass ionomer restorative material. J Am Dent Assoc 1995;
126:1245-1253.
2. Dentsply XP BOND for eXtra Performance. Scientific Compendium. Kon-
stanz: Dentsply DeTrey, 2006.
3. Dondi Dall'Orologio G. 6-Month report: clinical evaluation of the adhesive
XP BOND for restoration of cervical lesions at the University of Bologna,
Italy. Report to Dentsply 2006.
4. Harnirattisai C, Inokoshi S, Shimada Y, Hosoda H. Adhesive interface be-
tween resin and etched dentin of cervical erosion/abrasion lesions. Oper
Dent 1993;18:138-143.
5. Kanca J. Resin bonding to wet substrate. I. Bonding to dentin. Quintes-
sence Int 1992;23:39-41.
6. Kanca J. Wet bonding: effect of drying time and distance. Am J Dent
1996; 9:273-276.
7. Loguercio AD, Reis A, Barbosa AN, Roulet JF. Five-year double-blind ran-
domized clinical evaluation of a resin-modified glass ionomer and a poly-
acid-modified resin in noncarious cervical lesions. J Adhes Dent 2003;
5:323-332.
8. Peireira GDS, da, Paulillo LAMS, de Goes MF, Dias CTS. How wet should
dentin be? Comparison of methods to remove excess water during moist
bonding. J Adhes Dent 2001;3:257-264.
9. Peumans M, Kanumilli P, De Munck J, Van Landuyt K, Lambrechts P, Van
Meerbeek B. Clinical effectiveness of contemporary adhesives: a system-
atic review of current clinical trials. Dent Mater 2005;21:864-881.
10. Sakoolnamarka R, Burrow MF, Prawer S, Tyas MJ. Micromorphological in-
vestigation of noncarious cervical lesions treated with demineralizing
agents. J Adhes Dent 2000;2:279-287.
11. Tay FR, Kwong SM, Itthagarun A, King NM, Yip HK, Moulding KM, Pashley
DH. Bonding of a self-etching primer to non-carious cervical sclerotic
dentin: Interfacial ultrastructure and microtensile bond strength evalua-
tion. J Adhes Dent 2000;2:9-28.
12. Tay FR, Pashley DH. Resin bonding to cervical sclerotic dentin: a review. J
Dent 2004;32:173-196.
13. Van Meerbeek B, Perdigao J, Lambrechts P, Vanherle G. The clinical per-
formance of adhesives. J Dent 1998;26:1-20.

268 The Journal of Adhesive Dentistry

Adhesive Luting Revisited: Influence of Adhesive,
Temporary Cement, Cavity Cleaning, and Curing Mode
on Internal Dentin Bond Strength
Roland Frankenbergera/Ulrich Lohbauerb/Michael Taschnerc/Anselm Petscheltd/
Sergej A. Nikolaenkoe

Purpose: To evaluate microtensile bond strength to Class I cavity floor dentin beneath adhesive inlays that were luted
with different adhesives, temporary cements, cleaning methods, and curing modes.

Materials and Methods: Occlusal cavities (4 x 4 mm, depth 3 mm) were prepared in 96 extracted human third mo-
lars. One part of the cavities was temporized with different temporary cements, which were removed after one week
using three techniques (scaler or air polishing with Prophypearls or ClinPro powder). Direct resin composite inlays
(Clearfil AP-X) were then placed with the luting composite Calibra using three adhesives (XP BOND/SCA, Syntac, Opti-
Bond FL). Teeth were cut into beams and after 24 h of water storage at 37°C, the sticks were subjected to microten-
sile bond strength evaluation. Samples were subjected to SEM fractographic analysis of failed interfaces.

Results: Contamination with temporary cement reduced dentin bond strengths (p < 0.05). Removing remnants of ce-
ments with Prophypearls air polishing resulted in the lowest bond strengths (p < 0.05). Separate light curing of the ad-
hesives did not produce higher dentin bond strengths (p > 0.05). Syntac still worked when Heliobond was omitted (p >
0.05). Immediate dentin sealing prior to temporizing increased internal bond strength (p < 0.05).

Conclusion: The dual-cured adhesive provided higher internal bond strengths between adhesive inlays and dentin. Con-
tamination of dentin with temporary cements is a hazard for excellent dentin adhesion of adhesive inlays. Therefore, im-
mediate dentin sealing and resin coating is promising.

Keywords: etch-and-rinse, dentin bonding, adhesive inlays, microtensile bond strength.

J Adhes Dent 2007; 9: 269-273. Submitted for publication: 15.12.06; accepted for publication: 5.1.07.

a Associate Professor, Dental Clinic 1, Operative Dentistry and Periodontology,

University of Erlangen-Nuremberg, Erlangen, Germany.
b Assistant Professor, Dental Clinic 1, Operative Dentistry and Periodontology,
University of Erlangen-Nuremberg, Erlangen, Germany.
c Assistant Professor, Dental Clinic 1, Operative Dentistry and Periodontology,
University of Erlangen-Nuremberg, Erlangen, Germany.
d Professor and Chairman, Dental Clinic 1, Operative Dentistry and Periodon-
tology, University of Erlangen-Nuremberg, Erlangen, Germany.
e Professor and Head, Department of Operative Dentistry, Krasnojarsk State
Medical Academy, Krasnojarsk, Russia.
Paper presented at Satellite Symposium on Dental Adhesives, Dublin,
September 13th, 2006.
Reprint requests: Prof. Dr. Roland Frankenberger, Dental Clinic 1, Operative
Dentistry and Periodontology, University of Erlangen-Nuremberg, Glueckstrasse
11, D-91054 Erlangen, Germany. Tel: +49-9131-853-3693, Fax: +49-9131-853-
A dhesive inlays have proven to be durable in the oral cav-
ity.4,6,15,18,19,24,25,27,28 Clinical reports refer to bulk frac-
tures as the main failure reason for all ceramic inlay sys-
tems.8-10,15,18,19,26 Clinical trials focusing on ceramic inlays
reveal a certain deterioration of marginal quality;7 however,
when adhesive inlays are totally bonded to enamel and
dentin, internal dentin bond strength is also an interesting
factor for both stabilization and reduction of postoperative
hypersensitivity.14,15,20
It is still not fully understood which mode of luting is most
reliable for bonding adhesive tooth-colored inlays to enam-
el and dentin, but conventional etch-and-rinse systems with
dual-cured resin composites seem to be the gold standard
for luting.1,15,18,20,16
Therefore, the aim of the present in vitro study was to eval-
uate the performance of different etch-and-rinse adhesives

Vol 9, Supplement 2, 2007 269

Frankenberger et al

Table 1 Overview of materials under investigation

Adhesive + Components Manufacturer

resin composite

XP BOND/SCA + Etchant: 36% phosphoric acid Dentsply DeTrey; Konstanz,

Calibra Primer/Bond: TCB resin, PENTA, UDMA, TEG-DMA, BHT, CQ, functionalized Germany
nanofiller; mixed with SCA (self-curing activator)
Luting composite:
Base: bis-GMA, EBPADM, silica, UDMA, TEG-MA, butylhydoxitoluol, barium
glass, silica
Catalyst: bis-GMA, EBPADM, silica, UDMA, TEG-MA, butylhydoxitoluol, benzoyl
peroxide, barium glass, silica

Syntac Etchant: 35% phosphoric acid Ivoclar Vivadent; Schaan,

(with Calibra) Primer: maleic acid 4%, TEG-DMA, water, acetone Liechtenstein
Adhesive (2nd primer): water, PEG-DMA, glutaraldehyde
Heliobond: bis-GMA, UDMA, TEG-DMA
Luting composite: see above

OptiBond FL Etchant: 37.5% phosphoric acid Kerr; Orange, CA, USA

(with Calibra) Primer: HEMA, GPDM, MMEP, ethanol, water, initiators
Adhesive: bis-GMA, HEMA, GPDM, barium-aluminum borosilicate glass,
disodium hexafluorosilicate, fumed silica (total=48% filler)
Luting composite: see above

for luting of Class I resin composite inlays after different
contaminations, temporary cement removal, and curing
modes. The null hypothesis was twofold, that (1) different
adhesives with different curing modes, and (2) different
temporary cements and cleaning methods would have no
influence on dentin bond strength beneath adhesively lut-
ed inlays.
MATERIALS AND METHODS
Ninety-six intact, noncarious, unrestored human third mo-
lars were stored in an aqueous solution of 0.5% chlora
mine T at 4°C for up to 30 days. The teeth were debrided of
residual plaque and calculus, and examined to ensure that
they were free of defects under a light microscope at 20X
magnification. Standardized Class I cavity preparations (4
mm in width and length, 3 mm in depth) were performed.
Cavities were cut using coarse diamond burs under profuse
water cooling (80 μm, Two-Striper Prep-Set, Premier; St Paul,
MN, USA), and finished with a 25-μm finishing diamond. In-
ner angles of the cavities were rounded and the margins
were not bevelled. To guarantee a rectangular relation be-
tween the bonded interface and the direction of the later-cut
μTBS beam, the cusps were flattened by 2 mm and then the
cavity floor was prepared parallel to the flattened cusps.
Direct resin composite inlays (Clearfil AP-X, Kuraray;
Tokyo, Japan) were manufactured under isolation of the cav-
ities with glycerine gel. The inlays received a cubic shape
with the surface being parallel to the bottom of the cavity to
facilitate positioning of the light-curing tip. The bottom sides
of the inlays were sandblasted with aluminum oxide (Rond-
oflex 27 μm, KaVo; Biberach, Germany), washed with 70%
ethanol, and dried. The prepared teeth received provisional
restorations (Fermit N, Ivoclar Vivadent; Schaan, Liechten-
stein), and were stored in distilled water at 37°C for one
week. The provisional restorations were either inserted with
or without two different temporary cements (Temp Bond /
Temp Bond NE, Kerr; Orange, CA, USA). Two more groups
with hybridizing dentin prior to temporizing were also made,
either with one coat of adhesive (immediate dentin sealing17
[IDS]) or with one 0.5-mm layer of flowable resin composite
(X-Flow, Dentsply DeTrey; Konstanz, Germany) (resin coating
technique13 [RC]). Here, temporary cements were omitted
because they play no role in bonding to dentin.
After removing Fermit, cement remnants were removed
with a scaler or using different air-polishing powders (Pro-
phypearls Powder, KaVo; ClinPro Prophy Powder, 3M ESPE;
Seefeld, Germany), both operating in a Prophyflex air-pol-
ishing device (KaVo) at the level of the occlusal cavity mar-
gin for 10 s.2 After rinsing with tap water and drying, the cav-
ities were treated with different adhesives and one luting
composite (Table 1). Internal surfaces of the resin compos-
ite inlays were silanized with Monobond S (Ivoclar Vivadent),
dried, and covered with the respective adhesive, which was
not light cured. Adhesives and luting resin composite were
polymerized with a Translux CL light-curing unit (Heraeus
Kulzer; Dormagen, Germany). The intensity of the light was
checked periodically with a radiometer (Demetron Research;
Danbury, CT, USA) to ensure that 600 mW/cm2 was always
exceeded during the experiments. Adhesives were light
cured for 40 s in the case where the protocol advised it. Oth-

270 The Journal of Adhesive Dentistry

 Frankenberger et al

Table 2 Results of μTBS investigation to cavity floor dentin

Adhesive Dentin Cleaning Curing mode μTBS

contamination method of adhesive to cavity floor
dentin in MPa (SD)

XP BOND / SCA --- --- No LC 39.6 (26.6)

--- --- separate 36.3 (19.2)
--- --- IDS 38.4 (13.6)
--- --- RC 53.9 (17.1)
Temp Bond Scaler no LC 21.9 (20.7)
Temp Bond Prophypearls no LC 10.0 (14.9)
Temp Bond Clinpro powder no LC 34.5 (8.1)
Temp Bond NE Scaler no LC 27.3 (16.2)
Temp Bond NE Prophypearls no LC 11.0 (14.9)
Temp Bond NE Clinpro powder no LC 36.3 (20.5)

Syntac --- --- No LC 13.7 (15.7)

--- --- separate 19.0 (14.2)
--- --- IDS 30.1 (15.9)
--- --- RC 47.9 (18.0)
--- --- w/o adhesive 22.5 (14.3)
Temp Bond Scaler no LC 9.7 (8.9)
Temp Bond Prophypearls no LC 5.9 (6.5)
Temp Bond Clinpro powder no LC 12.1 (11.4)
Temp Bond NE Scaler no LC 7.1 (10.3)
Temp Bond NE Prophypearls no LC 4.1 (5.1)
Temp Bond NE Clinpro powder no LC 12.0 (8.9)

OptiBond FL --- --- No LC 19.2 (16.3)

--- --- separate 26.6 (13.8)
--- --- IDS 37.7 (16.9)
--- --- RC 50.7 (17.8)
--- --- w/o adhesive 24.0 (17.5)
Temp Bond Scaler no LC 10.4 (9.5)
Temp Bond Prophypearls no LC 6.5 (6.5)
Temp Bond Clinpro powder no LC 18.2 (12.6)
Temp Bond NE Scaler no LC 8.3 (10.2)
Temp Bond NE Prophypearls no LC 8.2 (10.5)
Temp Bond NE Clinpro powder no LC 22.1 (18.0)

IDS=immediate dentin sealing; RC=resin-coating technique

erwise, the luting composites were cured together with the
adhesives with an occlusal curing time of 220 s.
The peripheral areas of the reconstructed/filled teeth
were removed, remaining specimens were sectioned into
slices in an apical direction, which were sectioned again to
yield resin-dentin beams. The saw was adjusted to steps of
1 mm, due to the thickness of the blade (300 μm) resulting
in sticks with a cross-sectional area of 700 x 700 μm (0.5
mm2). From the resulting sticks of each group, 20 were se-
lected (n = 20). These 20 sticks had to have a remaining
dentin thickness to the pulp of 2.0 ± 0.5 mm. If more than
20 beams were collected with the correct remaining dentin
thickness, 20 sticks were randomly selected. For the case
that one or more of the selected sticks failed due to the sec-
tioning process, the percentage of prematurely failed spec-
imens in relation to the total number of selected specimens
was recorded. If more than 20 beams were collected with
the correct remaining dentin thickness, 20 sticks were ran-
domly selected. For the case that one or more of the select-
ed sticks failed due to the sectioning process, the failed
specimens received 0 MPa as final μTBS result.38 The μTBS
sticks were stored in distilled water for 24 h at 37°C and then
fractured according to a well-suited protocol.3 Fractured in-
terfaces were submitted to SEM (Leitz ISI 50, Akashi; Tokyo,
Japan; sputtering with Balzers SCD; Balzers, Liechtenstein).
Statistical analysis was performed using SPSS, Version
14.0 for Windows XP (SPSS; Chicago, IL, USA). As the ma-
jority of groups did not exhibit normal data distribution (Kol-
mogorov-Smirnov test), nonparametric tests were used
(Wilcoxon matched-pairs signed-ranks test, Mann-Whitney
U-test) for pairwise comparisons at the 95% significance
level.

Vol 9, Supplement 2, 2007 271

Frankenberger et al
Fig 1 Fractured μTBS specimen at the resin composite aspect
with Syntac not separately cured. Short resin tags have been
pulled out of the dentin at the cavity floor.
RESULTS
The results of the study are displayed in Table 2. Contami-
nation with temporary cement reduced dentin bond
strengths (p < 0.05). Removing remnants of cements with
Prophypearls air-polishing significantly decreased dentin
bond strengths (p < 0.05). Separate light curing of the ad-
hesives did not produce higher dentin bond strengths (p >
0.05). The dual-cured adhesive exhibited significantly high-
er bond strengths in control groups without IDS (p < 0.05).
Immediate dentin sealing (resin coating) prior to temporizing
increased internal bond strength for all adhesives under in-
vestigation (p < 0.05). Fractographic analysis exhibited in-
sufficient interface formation when light-cured adhesives
were cured together with the luting resin composite (Fig 1).
Fractured interfaces of XP Bond showed characteristic pos-
itive features of typical etch-and-rinse adhesives (Fig 2).
DISCUSSION
The survival of ceramic inlays is fundamentally dependent
on durable enamel bonding; also when the dentin aspects
were covered with a cement lining, long-term success was re-
ported to be good.4,14-16 However, the present study exclu-
sively focussed on internal dentin bond strength beneath ad-
hesive inlays. Due to easier processing, direct resin com-
posite inlays were chosen, because they reveal the same
dentin-resin composite interface as ceramic inlays.12,13,16,29
Hikita et al11 evaluated enamel and dentin bond
strengths of luting systems for adhesive inlays. It was re-
markable that Syntac and Variolink II without separate light
curing of the adhesive obtained the lowest dentin bond
strengths in that investigation. This may be surprising, be-
cause especially this combination of light-curing adhesive
and dual-curing luting resin composite has been repeatedly
272
Fig 2 Fractured μTBS specimen with XP Bond + SCA at the
dentin side. The interface is ruptured at the bottom of the hybrid
layer at the transition to the funnel-shaped orifices of dentinal
tubules.
reported to be clinically effective.4,14,15 This clearly demon-
strates that the clinical success of ceramic inlays as well as
of direct resin composite restorations may be primarily de-
pendent on good and durable marginal adaptation to enam-
el. The present results also clearly confirm the theory that
solely light-cured adhesives do not receive enough light en-
ergy through 3-mm-thick adhesive inlays, not even under lab-
oratory conditions. To elucidate the problem of insufficient
light curing through ceramic inlays as demonstrated in vitro,
marginal quality assessment alone is not sufficient. A previ-
ous and often cited study with conical ceramic inserts luted
into standardized dentin cavities showed good bond
strengths and marginal adaptation in vitro, even when the
light-curing adhesive was not light cured separately.5 How-
ever, in the course of push-out investigations, in most of the
cases, enough light energy passes through the specimens,
being considerably thinner than inlay cavities. Previous re-
sults showed that enough light intensity was always trans-
ported to the marginal areas of the luted ceramic inays,
even in proximal margins below the CEJ.1 Nevertheless, this
does not necessarily mean that the light-curing adhesives
under investigation revealed a complete cure in all areas be-
neath the ceramic inlays. The present results clearly show
that results of marginal analyses may produce results which
are not representative for what is happening deeper inside
the restored tooth.
In this context, it has often been discussed in the past
whether a light-cured adhesive has to be separately light
cured prior to the application of a luting resin composite.
This study indicates that a separate light-curing step of light-
cured adhesives was not beneficial for dentin bond strength.
This may be attributed to the fact that heavily air-thinned lay-
ers of bonding agents are subjected to severe oxygen inhi-
bition and are therefore almost not cured despite the pres-
ence of light energy for 40 s. Finally, due to reasons of con-
tamination and oxygen inhibition, immediate dentin sealing
The Journal of Adhesive Dentistry

or resin coating may be the method of choice to pretreat
dentin surfaces being chosen for adhesive luting, because
contamination with temporary cements is avoided and ap-
propriate polymerization of the resin-dentin interface is guar-
anteed.12,13,17,21,23,29 This is given even more credence, be-
cause the present study was able to demonstrate that any
contamination with temporary cements is crucial, and re-
moval methods such as air polishing are sometimes disad-
vantageous, as proven in a previous investigation conduct-
ed with the effect of air-polishing alone.2 Finally, both null hy-
potheses had to be rejected.
CONCLUSIONS
The dual-cured adhesive provided higher internal bond
strengths to dentin beneath adhesive inlays. Contamination
of dentin with temporary cements is a hazard for excellent
dentin adhesion of adhesive inlays. Therefore, immediate
dentin sealing is promising. Among temporary cement clean-
ing techniques, polishing air abrasion with Prophypearls se-
verely reduces dentin bond strengths.
REFERENCES
1. Frankenberger R, Lohbauer U, Schaible BR, Nikolaenko SA, Naumann M.
Luting of ceramic inlays in vitro: marginal quality of self-etch and etch-and-
rinse adhesives vs. self-etch cements. Dent Mater 2006;submitted.
2. Frankenberger R, Lohbauer U, Tay FR, Taschner M, Nikolaenko SA. Air-pol-
ishing powders differently affect dentin bonding. J Adhes Dent 2007;
accepted for publication.
3. Frankenberger R, Pashley DH, Reich SM, Lohbauer U, Petschelt A, Tay FR.
Characterisation of resin-dentine interfaces by compressive cyclic loading.
Biomaterials 2005;26:2043-2052.
4. Frankenberger R, Petschelt A, Krämer N. Leucite-reinforced glass ceramic
inlays and onlays after six years: clinical behavior. Oper Dent
2000;25:459-465.
5. Frankenberger R, Sindel J, Krämer N, Petschelt A. Dentin bond strength
and marginal adaptation: direct composite resins vs ceramic inlays. Oper
Dent 1999;24:147-155.
6. Fuzzi M, Rappelli G. Ceramic inlays: clinical assessment and survival rate.
J Adhes Dent 1999;1:71-79.
7. Hayashi M, Tsubakimoto Y, Takeshige F, Ebisu S. Analysis of longitudinal
marginal deterioration of ceramic inlays. Oper Dent 2004;29:386-391.
8. Hayashi M, Tsuchitani Y, Kawamura Y, Miura M, Takeshige F, Ebisu S. Eight-
year clinical evaluation of fired ceramic inlays. Oper Dent 2000;25:473-
481.
9. Hayashi M, Wilson NH, Yeung CA, Worthington HV. Systematic review of ce-
ramic inlays. Clin Oral Investig 2003;7:8-19.
10. Hayashi M, Yeung CA. Ceramic inlays for restoring posterior teeth. Aust
Dent J 2004;49:60.
Vol 9, Supplement 2, 2007
Frankenberger et al
11. Hikita K, Van MB, De MJ, Ikeda T, Van LK, Maida T, Lambrechts P, Peu-
mans M. Bonding effectiveness of adhesive luting agents to enamel and
dentin. Dent Mater 2006.
12. Islam MR, Takada T, Weerasinghe DS, Uzzaman MA, Foxton RM, Nikaido T,
Tagami J. Effect of resin coating on adhesion of composite crown restora-
tion. Dent Mater J 2006;25:272-279.
13. Jayasooriya PR, Pereira PN, Nikaido T, Tagami J. Efficacy of a resin coating
on bond strengths of resin cement to dentin. J Esthet Restor Dent
2003;15:105-113.
14. Krämer N, Ebert J, Petschelt A, Frankenberger R. Ceramic inlays bonded
with two adhesives after 4 years. Dent Mater 2006;22:13-21.
15. Krämer N, Frankenberger R. Clinical performance of bonded leucite-rein-
forced glass ceramic inlays and onlays after eight years. Dent Mater
2005;21:262-271.
16. Krämer N, Lohbauer U, Frankenberger R. Adhesive luting of indirect
restorations. Am J Dent 2000;13:60D-76D.
17. Magne P, Kim TH, Cascione D, Donovan TE. Immediate dentin sealing im-
proves bond strength of indirect restorations. J Prosthet Dent 2005;
94:511-519.
18. Manhart J, Chen H, Hamm G, Hickel R. Buonocore Memorial Lecture. Re-
view of the clinical survival of direct and indirect restorations in posterior
teeth of the permanent dentition. Oper Dent 2004;29:481-508.
19. Martin N, Jedynakiewicz NM. Clinical performance of CEREC ceramic in-
lays: a systematic review. Dent Mater 1999;15:54-61.
20. Mehl A, Kunzelmann KH, Folwaczny M, Hickel R. Stabilization effects of
CAD/CAM ceramic restorations in extended MOD cavities. J Adhes Dent
2004;6:239-245.
21. Nikaido T, Cho E, Nakajima M, Tashiro H, Toba S, Burrow MF, Tagami J. Ten-
sile bond strengths of resin cements to bovine dentin using resin coating.
Am J Dent 2003;16 Spec No:41A-46A.
22. Nikolaenko SA, Lohbauer U, Roggendorf M, Petschelt A, Dasch W, Franken-
berger R. Influence of c-factor and layering technique on microtensile bond
strength to dentin. Dent Mater 2004;20:579-585.
23. Ozturk N, Aykent F. Dentin bond strengths of two ceramic inlay systems
after cementation with three different techniques and one bonding sys-
tem. J Prosthet Dent 2003;89:275-281.
24. Pallesen U, van Dijken JW. An 8-year evaluation of sintered ceramic and
glass ceramic inlays processed by the Cerec CAD/CAM system. Eur J Oral
Sci 2000;108:239-246.
25. Posselt A, Kerschbaum T. Longevity of 2328 chairside Cerec inlays and on-
lays. Int J Comput Dent 2003;6:231-248.
26. Reiss B. Clinical results of Cerec inlays in a dental practice over a period of
18 years. Int J Comput Dent 2006;9:11-22.
27. Schulz P, Johansson A, Arvidson K. A retrospective study of Mirage ceramic
inlays over up to 9 years. Int J Prosthodont 2003;16:510-514.
28. Sjögren G, Molin M, van Dijken JW. A 10-year prospective evaluation of
CAD/CAM-manufactured (Cerec) ceramic inlays cemented with a chemi-
cally cured or dual-cured resin composite. Int J Prosthodont 2004;17:241-
246.
29. Stavridakis MM, Krejci I, Magne P. Immediate dentin sealing of onlay
preparations: thickness of pre-cured dentin bonding agent and effect of
surface cleaning. Oper Dent 2005;30:747-757.
Clinical relevance: Dual-cured adhesives are beneficial
for adhesive luting. Sealing dentin prior to temporizing
improves dentin bond strength.
273
Sarrett

274 The Journal of Adhesive Dentistry

XP BOND in Self-curing Mode used for Luting Porcelain
Restorations. Part A: Microtensile Test
Ornella Raffaellia/Maria Crysanti Cagidiacob/Cecilia Goraccic /Marco Ferrarid

Purpose: To assess the bond strength to dentin of an experimental adhesive and the proprietary resin cement used
in different curing modes to lute ceramic disks of different thicknesses.

Materials and Methods: Empress II disks (Ivoclar-Vivadent) were luted to dentin using XP BOND (Dentsply [XP]) in
combination with the proprietary self-curing activator (SCA) and cement Calibra (Dentsply [C]). Curing of the adhesive
was induced either by mixing with the activator (activator, groups 3 to 6) or by light irradiation for 20 s (group 2). The
cement was either light cured for 40 s through the ceramic onlay (groups 1 to 5) or cured chemically (groups 6 and 7).
Groups 2 and 4 were compared with group 1, in which Prime & Bond NT (Dentsply DeTrey) was tested as control. In
groups 3 and 6, 2-mm-thick onlays were luted with XP+SCA, and the cement was light cured for 40 s or let autocure for
5 min, respectively. These groups were compared with group 7, in which Syntac (Ivoclar Vivadent) was applied with C
and, in order to reproduce the handling procedures of group 6 (although contrary to manufacturer’s instructions), no
light irradiation was provided for the adhesive or the cement. The influence of onlay thickness (2, 3, 4 mm) on the
bond strength developed by XP+SCA/C was assessed by comparing groups 3, 4, 5. In these groups, C was light cured
for 40 s through the onlay. Microtensile beams were obtained from the luted teeth.

Results: Bond strengths not including pretest failures (in parentheses: value including pretest failures as 0 MPa) were
21.0 (17.5) MPa in group 1, 24.9 (21.2) MPa in group 2, 23.7 (21.3) MPa in group 3, 29.9 (26.7) MPa in group 4, 30.3
(24.6) MPa in group 5, 28.6 (24.6) MPa in group 6, and 17.1 (9.2) MPa in group 7. Statistically significant differences
were found between groups 1 and 4, groups 3 and 5, and groups 6 and 7.

Conclusion: The bonding potential of XP BOND used with the activator or light cured in combination with Calibra in
self- or dual-curing mode outperformed that of a control adhesive-cement system. The bond strength of XP+ SCA + Cal-
ibra was not negatively affected by the onlay thickness.

J Adhes Dent 2007; 9: 275-278. Submitted for publication: 15.12.06; accepted for publication: 5.1.07.

M any new bonding systems are introduced every year on

the market. Some of them are primer-adhesive solu-
tions in combination with a prior phosphoric acid treatment,
others avoid the total-etch step and offer self-etching or self-
adhesive bonding solutions.3,5,7-10
However, practitioners would like to use the same bond-
ing systems for all clinical applications, although most sim-
a PhD Student, Department of Dental Materials and Prosthodontics, University of
Siena, Siena, Italy.
b Clinical Professor of Dentistry, Department of Dental Materials and Prostho-
dontics, University of Siena, Siena, Italy.
c Assistant Professor and Chair, Department of Endodontics, University of Siena,
Siena, Italy.
d Professor and Chair, Department of Dental Materials and Prosthodontics, Uni-
versity of Siena, Siena, Italy.
Paper presented at Satellite Symposium on Dental Adhesives, Dublin,
September 13th, 2006.
Reprint requests: Prof. Marco Ferrari, Research Center for Dental Health, 19 Pi-
azza Attias, 57120 Livorno, Italy. Tel: +39-586-892-283, Fax: +39-586-898-305.
e-mail: ferrarimar@unisi.it
plified bonding solutions are not necessarily indicated for
luting indirect restorations, limiting their clinical indications
to direct restorations.
Recently, XP BOND (Dentsply DeTrey; Konstanz, Ger-
many), using tert-butanol for the first time as solvent in den-
tistry, was proposed as a one-bottle universal adhesive, al-
so in combination with a new self-curing activator (SCA).
When luting a porcelain restoration, differences in thick-
ness may reduce the light penetration, resulting in a re-
duced polymerization rate of the luting material.1,2,4 To avoid
an incomplete cure of the resin cement adhesive interface,
the self-curing activator can be used.
Consequently, the aims of this study were to evaluate (1)
the procedure for adhesively luting ceramic to dentin and,
specifically, when light is applied, to cure either the adhesive
before or after applying the cement, (2) the influence of ce-
ramic thickness when the adhesive is not separately light
cured but mixed with a self-curing activator (SCA), (3) the in-
fluence of SCA on the bonding efficacy when no light is
used. The null hypothesis tested is that differences in porce-
lain thickness and curing mode do not affect the bond
strength values.

Vol 9, Supplement 2, 2007 275

Raffaelli et al

Table 1 Groups of materials and techniques

Groups Adhesive Activator Adhesive Cement Ceramic disk

thickness (mm)

1 Prime & Bond NT no LC DC 3

2 XP BOND no LC DC 3
3 XP BOND yes NC DC 2
4 XP BOND yes NC DC 3
5 XP BOND yes NC DC 4
6 XP BOND yes NC CC 2
7 Syntac* - NC CC 2

NC: not cured (mix with SCA is applied, but not light cured); LC: light cured (light cured before placement); DC: dual curing (Light is applied on the mixed
cement); CC: chemically cured (no light is used at all). *According to the directions for use, application and light curing of Heliobond is mandatory when com-
bined with self curing materials.

MATERIALS AND METHODS TBS Evaluation and SEM Fractographic Analysis

Bonding was performed on 70 noncarious human third mo-
lars that were extracted after informed consent had been ob-
tained. They were stored in a 1% chloramine T solution at
4°C and used within one month following extraction. Prior to
the bonding experiments, the teeth were retrieved from the
disinfectant solution and stored in distilled water, with four
changes of the latter within 48 h to remove the disinfectant.
Tooth Preparation – Bonding to Deep Dentin
Bonding was performed on the occlusal surfaces of deep
coronal dentin. The occlusal enamel and the superficial
dentin of each tooth were removed using a slow-speed saw
(Isomet, Buehler; Lake Bluff, IL, USA) under water cooling.
The tooth surfaces were polished with wet 180-grit SiC pa-
pers. The teeth were divided into 7 experimental groups of
10 teeth each. The experimental dentin groups are listed in
Table 1.
Coupling of Processed Ceramic
Empress 2 blocks (shade A2) were reduced with the Isomet
saw under water cooling to produce blocks with dimensions
similar to those of the teeth to be bonded. Each reduced
block was then sectioned with the Isomet saw to produce
2-, 3-, or 4-mm-thick, parallel-sided ceramic onlays. The in-
ner surface of each ceramic onlay was sandblasted with 50-
μm alumina, etched with a hydrofluoric acid gel for 90 s,
washed, air dried, and silanized using Calibra silane
(Dentsply).
To bond the ceramic disks to the dentin surface, the
bonding systems and the resin cement were used following
manufacturer’s instructions. As a curing device, a QTH light
(Dentsply DeTrey) was used (power output: 800 mW/cm2).
The intensity of the curing light was tested before and after
curing with a radiometer. The bonded specimens were
stored in distilled water at 37°C for 24 h before further lab-
oratory processing.
Each tooth was sectioned occluso-gingivally into serial slabs
using an Isomet saw under water cooling. The two slabs from
each tooth were further sectioned into 0.9 x 0.9 mm ce-
ramic-dentin beams, according to the technique for the
nontrimming version of the microtensile test.6 Each group
provided 37 to 53 beams for bond strength evaluation. Pre-
mature failures that occurred during sectioning were record-
ed. The specimens were stressed to failure under tension us-
ing a universal testing machine (Model 4440, Instron; Can-
ton, MA, USA) at a crosshead speed of 1 mm/min. The data
were analyzed using one-way ANOVA and Tukey’s multiple
comparison tests at α = 0.05.
Representative fractured beams from each of the 7
groups were air dried and sputter coated with gold/palladi-
um for examination with a conventional SEM (Jeol; Tokyo,
Japan).
Statistical Analysis
Three different one-way ANOVAs were performed, each in-
volving different groups (Tables 2 to 4). The first two analy-
ses were performed in the groups with 3-mm and 2-mm ce-
ramic disks, respectively. The last analysis was performed
on groups with 3 different ceramic thicknesses (2, 3, and 4
mm) when samples were luted with XP+SCA+Calibra DC.
Premature failures were excluded from the statistical analy-
sis. It was also verified that the tooth of origin was not a sig-
nificant factor for bond strength.
As the bond strength data were normally distributed (Kol-
mogorov-Smirnov test) and groups had homogeneous vari-
ances (Levene test), one-way ANOVA was applied to test for
significance of differences among the tested groups, fol-
lowed by Tukey’s test for post-hoc comparisons. In all the
analyses, the level of significance was set at α = 95%.
RESULTS
The bond strength values found in this investigation are re-
ported in Fig 1 and Tables 2 to 4.

276 The Journal of Adhesive Dentistry

 Raffaelli et al

Table 2 Bond strength values obtained luting 3-mm-thick
porcelain disks. n=sample size (in parentheses, number
of premature failures), mean, and standard deviation (SD)
values excluding premature failures. Premature failures
were excluded from the statistical analysis
Table 3 Bond strength values obtained luting 2-mm-thick
porcelain disks. n=sample size (number of premature fail-
ures in parentheses), mean and standard deviation (SD)
values excluding premature failures. Premature failures
were excluded from the statistical analysis

Group N Mean (MPa) SD Group N Mean (MPa) SD

1. (control): 42 (7) 20.9BC 10 3. XP+ SCA + 35 (4) 23.6AB 11.1

PBNT LC + Calibra DC
Calibra DC
6. XP + SCA + 37 (6) 28.6A 10.4
2. XP LC + 53 (8) 24.9AB 10.7 Calibra CC
Calibra DC
7. Syntac No LC 20 (17) 17.1B 6.6
4. XP + SCA + 37 (4) 29.8A 12.9 + Calibra CC
Calibra DC
According to the post-hoc test, XP+SCA (No LC)+Calibra CC achieved a
According to the post-hoc test, XP+SCA+Calibra DC achieved a signifi- significantly higher bond strength than Syntac No LC+Calibra CC.
cantly higher bond strength than group 1. Groups with the same upper- Groups with the same uppercase letter are not statistically significantly
case letter are not statistically significantly different. different.

Table 4 Bond strength values recorded using 3 different porcelain thicknesses.

n=sample size (number of premature failures in parentheses), mean and standard
deviation values excluding premature failures. Premature failures were excluded
from the statistical analysis

Ceramic Adhesive/ n Mean (MPa) SD

thickness resin cement

Group 3: XP+SCA+Calibra 35 (4) 23.6B 11.1

2 mm DC

Group 4:
3 mm 33 (4) 29.8AB 12.1

Group 5:
4 mm 43 (10) 30.3A 12.3

According to the post-hoc test, the bond strengths measured with 4-mm-thick disks were significantly
higher than those measured with 2-mm-thick disks. Groups with the same uppercase letter are not sta-
tistically significantly different.

Groups 4, 5, and 6 showed the highest bond strength val- DISCUSSION

ues. In these three groups, the XP BOND was not light cured
before seating the ceramic onlay, and in group 6 Calibra was
chemically cured. When comparing the groups that differed
in ceramic onlay thickness, it was noted that the specimens
obtained from 4-mm-thick onlays (group 5) showed the high-
est bond strength but also a higher percentage of pretest
failure.
SEM observations showed that adhesive fracture was
the most common failure type in groups 2 to 7. Only in group
1 were two cohesive failures in dentin and two mixed failures
recorded.
The microtensile evaluation performed in this study was
used in order to standardize the bond strength test and eval-
uate two different variables, the restorative material thick-
ness and the curing mode of the adhesive-luting agent com-
binations. In order to properly apply the statistical analysis,
it was decided to report the number of premature failures in
the tables without including them in the analysis. Only in
group 7 was the number of premature failures rather high
(45%). In the other groups, the percentage of premature fail-
ures was 10% to 19%. The occurrence of premature failures
may be due to the stress transmitted at the bonding inter-
face during the specimen reparation procedure.

Vol 9, Supplement 2, 2007 277

Raffaelli et al
The results of this study demonstrated that the thickness
of the porcelain restoration does not affect the polymeriza-
tion of the adhesive/luting combination: in the three groups
(3 to 5) in which the thickness of porcelain disks was 2, 3,
and 4 mm, respectively, the bond strength values were be-
tween 23.6 and 30.3 MPa with a progressive increase of
bond strength proportional to the porcelain thickness. This
could be due to the efficacy of the self-curing mode of the
new bonding material and/or to the intrinsically greater
strength of thicker porcelain. This result should lay to rest
any doubts that a thick ceramic restoration cannot be luted
using a one-bottle system in combination with a resin ce-
ment.
The results also suggest that XP BOND can be considered
a proper bonding system for luting full and partial porcelain
crowns. In order to simplify the clinical luting procedures and
according to the results of this study, XP BOND and Calibra
resin cement can routinely be used in the self-curing mode.
A study on the clinical performance of XP BOND cured by the
application of its self-activator and used in combination with
Calibra resin cement is currently ongoing.
CONCLUSIONS
From the results of this study the following conclusions can
be drawn:
XP BOND can be used in the self-curing mode in combi-
nation with SCA and Calibra resin cement for luting porce-
lain restorations.
The porcelain restoration thickness is not a limitation to
the curing process of the adhesive-luting material combina-
tion when XP BOND is self-activated.
278
Fig 1 Bond strength values (without
premature failures) and percentage of
premature failures (ptf) of the seven
tested groups. NC: not cured; LC: light
cured; DC: dual cured; CC: chemically
cured.
ACKNOWLEDGMENTS
This research was sponsored by Dentsply DeTrey, Konstanz, Germany.
REFERENCES
1. Bergman MA. The clinical performance of ceramic inlays: a review. Aust Dent
J 1999;44:157-168.
2. Davidson CL. Luting cement, the stronghold or the weak link in ceramic
restorations. Adv Engineer Mater 2001;3:763-767.
3. De Munck J, Vargas M, Van Landuyt K, Hikita K, Lambrechts P, Van Meerbeek
B. Bonding of an auto-adhesive luting material to enamel and dentin. Dent
Mater 2004;20:963-971.
4. Hahn P, Schaller HG, Hafner P, Hellwig E. Effect of different luting procedures
on the seating of ceramic inlays. J Oral Rehabil 2000;27:1-8.
5. Pashley DH, Pashley EL, Carvalho RM, Tay FR. The effects of dentin perme-
ability on restorative dentistry. Dent Clin North Am 2002;46:211-245.
6. Shono Y, Terashita M, Shimada J, Kozono Y, Carvalho RM, Russell CM, Pash-
ley DH. Durability of resin-dentin bonds. J Adhes Dent 1999;1:211-218.
7. Tay FR, Frankenberger R, Krejci I, Bouillaguet S, Pashley DH, Carvalho RM,
Lai CN. Single-bottle adhesives behave as permeable membranes after poly-
merization. I. In vivo evidence. J Dent 2004;32:611-621.
8. Tay FR, Pashley DH, Suh BI, Hiraishi N, Yiu CK. Water treeing in simplified
dentin adhesives - déjà vu? Oper Dent 2005;30:561-579.
9. Tay FR, Pashley DH. Dental adhesives of the future. J Adhes Dent 2002;4:91-
103.
10. Van Meerbeek B, De Munck J, Yoshida Y, Inoue S, Vargas M, Vijay P, Van Lan-
duyt K, Lambrechts P, Vanherle G. Buonocore memorial lecture. Adhesion to
enamel and dentin: current status and future challenges. Oper Dent
2003;28:215-235.
Clinical relevance: The results of this microtensile inves-
tigation show good performance of XP BOND in its self-cur-
ing mode.
The Journal of Adhesive Dentistry
XP BOND in Self-curing mode used for Luting Porcelain
Restorations. Part B: Placement and 6-month Report
Marco Ferraria/Ornella Raffaellib/Maria Crysanti Cagidiacoc/Simone Grandinid

Purpose: The aim of this clinical study was to evaluate the postoperative sensitivity of Empress II restorations luted un-
der clinical conditions with XP BOND in combination with SCA and Calibra cured in self-curing mode.

Materials and Methods: Fifty-three restorations were placed in 38 patients in March and April 2006. No patient received
more than two restorations. Luting procedures were performed following manufacturers’ instructions. The restorations
were evaluated after 2 weeks and 6 months for postoperative sensitivity, marginal discoloration, marginal integrity, sec-
ondary caries, maintenance of interproximal contact, and fracture.

Results: At the 2-week recall, the postoperative sensitivity was reported in only 10 and after 6 months in only 3 patients.
All other parameters showed alpha scores.

Conclusion: All the evaluated restorations were in place and acceptable. The postoperative sensitivity recorded after
using XP BOND and Calibra in self-curing mode was clinically acceptable.

Keywords: ceramic crowns, self-curing, clinical trial, bonding.

J Adhes Dent 2007; 9: 279-282. Submitted for publication: 15.12.06; accepted for publication: 11.1.07.

I ndirect ceramic restorations are a valid alternative to direct

esthetic restorations and to porcelain-fused-to-metal
crowns. The prerequisite for application of full and/or partial
porcelain crowns is perfect bonding, which has to integrate
all parts into one coherent structure.6 Therefore, luting ma-
terial and technique as well as the substrate characteristics
represent the factors determining success.7
a Dean, Professor, and Chair, Department of Dental Materials and Prosthodon-
tics, University of Siena, Siena, Italy.
b PhD Student, Department of Dental Materials and Prosthodontics, University
of Siena, Siena, Italy.
c Assistent Professor, Department of Dental Materials and Prosthodontics, Uni-
versity of Siena, Siena, Italy.
d Chair, Assistent Professor, Department of Endodontics, University of Siena,
Siena, Italy.
Paper presented at Satellite Symposium on Dental Adhesives, Dublin,
September 13th, 2006
Reprint requests: Prof. Marco Ferrari, Research Center for Dental Health, 19
Piazza Attias, 57120 Livorno, Italy. Tel: +39-586-892-283, Fax: +39-586-898-
305. e-mail: ferrarimar@unisi.it
Different combinations of adhesive luting materials have
been tested, and dual-curing bonding systems are often the
first choice.3,5,8,12,14-16,18,19,21 Dual-curing bonding agents
permit polymerization of the adhesive materials and the
resin cement underneath a thick ceramic restoration. Re-
cently, XP BOND (Dentsply DeTrey; Konstanz, Germany) was
proposed and tested experimentally, showing interesting da-
ta when the adhesive was used in self-curing mode.20
Postoperative sensitivity is a common complication when
porcelain crowns are luted on vital teeth.9 The aim of the pre-
sent prospective clinical trial was to evaluate the early post-
operative sensitivity of Empress II restorations (Ivoclar-Vi-
vadent; Schaan, Liechtenstein), cemented under clinical
conditions with the adhesive system XP BOND/SCA and Cal-
ibra resin cement (Dentsply Caulk; Milford, DE, USA), both
used in self-curing mode.
MATERIALS AND METHODS
The sample consisted of 53 consecutively placed restora-
tions in 38 patients in need of one or two single units. Par-

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Ferrari et al

Table 1 Changes in pre- and postoperative sensitivities (1 = lowest, 10 = highest

sensitivity)
case XP Bond / SCA / Calibra [n]

Type of Pre- Postoperative Postoperative

restoration operative sensitivity sensitivity
sensitivity (2 weeks (6 months
after after
placement) placement)

1 Inlay (OD) 0 6 3
2 Inlay (MOD) 0 1 0
3 Inlay (MO) 0 1 0
4 2 onlays 2 0 0
5 Onlay 0 1 0
6 Inlay (MOD) 3 1 0
and onlay
7 Inlay (MO) 0 1 0
8 Onlay 4 1 0
9 Onlay 0 3 2
10 Inlay (MOD) 0 1 0
11 Inlay (MOD) 0 3 2

tial or full restoration was performed from the pool of pa-
tients accessing the department of Restorative Dentistry of
the University of Siena. Patients’ written consent to the trial
was obtained after having provided a complete explanation
of the aim of the study.
Inclusion and Exclusion Criteria
Males and females aged 18 to 60 years in good general and
periodontal health were included. Patients to whom the fol-
lowing factors applied were excluded from the clinical trial:
1. Under 18 years of age
2. Pregnancy
3. Disabilities
4. Prosthodontic restoration of tooth can be expected
5. Pulpitic, nonvital, or endodontically treated teeth
6. (Profound, chronic) periodontitis
7. Deep defects (< 1 mm from pulp) or pulp capping
8. Heavy occlusal contacts or history of bruxism
9. Systemic disease or severe medical complications
10. History of allergy to methacrylates
11. Rampant caries
12. Xerostomia
13. Lack of compliance
14. Language barriers
Test Stimuli and Assessment
Before applying the adhesive material, a pain measurement
was performed utilizing a simple pain scale based on the re-
sponse method. Response was determined to a 1-s appli-
cation of air from a dental unit syringe (at 40 to 65 psi at ap-
proximately 20°C), directed perpendicularly to the root sur-
face at a distance of 2 cm, and by tactile stimuli with a sharp
#5 explorer. The patient was asked to rate the perception of
the sensitivity experienced during this thermal/tactile stim-
ulation by placing a mark on a visual analog scale (VAS) be-
ginning at 0 and ending at 10 (where 0 = no pain and 10 =
excruciating pain). In order to translate these scores into
easily understood pain levels, a score of 0 was defined as
no pain, 1 to 4 as mild sensitivity (which was provoked by the
air blast), and 5 to 10 as strong sensitivity (which was spon-
taneously reported by the patient during drinking and eat-
ing). Only patients scoring low on the VAS were included in
the study, whereas high score cases were excluded based
on the assumption that irreversible pulp inflammation could
be sustaining the high sensitivity. The status of the gingival
tissues adjacent to the test sites was observed at baseline
and at each recall. Patients were recalled to our department
for testing postoperative sensitivity after 2 weeks and 6
months.
Clinical Procedure
For standardization purposes, the same operator performed
all the clinical procedures. Following anesthesia, the rubber-
dam was placed, all carious structures were excavated, and
any restorative material was removed. Preparation was per-
formed using conventional diamond burs in a high-speed
handpiece with no bevel on margins. The preparation design
was dictated by the extent of decay and pre-existing restora-
tions. The residual dentin thickness (RDT) was evaluated on
a periapical radiograph, and teeth with RDT thinner than 0.5
mm were excluded. After preparation, the impression of the
prepared tooth was taken and sent to the laboratory. A tem-
porary restoration was performed. One week later, the ce-
ramic restorations were luted. Luting procedures were per-
formed under rubbes-dam. The cavity preparation was
cleaned with a rotating brush and pumice, and then water

280 The Journal of Adhesive Dentistry

 Ferrari et al

Table 2 Performance criteria according to Ryge

Criteria and number of XP Bond

restorations evaluated after SCA alpha bravo charlie delta
6 months Calibra[n]

Marginal discoloration and 53 53 0 0 0

integrity
Secondary caries 53 53 0 0 0

Vitality test 53 53 0 0 0

Interproximal contacts 53 53 0 0 0

Retention 53 53 0 0 0

Fracture 53 53 0 0 0

sprayed and air dried carefully. 36% phosphoric acid gel was
then applied for 15 s on enamel margins, and then for oth-
er 15 s on dentin. The gel was removed with air spray and
the surface blown gently with an air syringe. One drop of XP
Bond was dispensed and mixed with one drop of self-curing
activator. Using a microbrush, all cavity walls were wet and
the adhesive material was left undisturbed for 20 s. After
that, the solvent was evaporated by thoroughly blowing with
air from an air syringe for 5 s. No light curing step was per-
formed. Calibra Esthetic Resin Cement base and catalyst in
similar amounts were mixed and applied on the cavity sur-
face. Then the restoration was placed in the cavity prepara-
tion, and resin cement excess was removed with a clean mi-
crobrush. The Calibra cement was used in self-curing mode.
The restorations were placed in March and April 2006 and
examined for postoperative sensitivity at baseline, after 2
weeks and 6 months by the same operator. At each recall,
data on postoperative sensitivity, stability, and longevity
were collected with reference to the USPHS criteria. There-
fore, the following parameters were assessed:
• postoperative sensitivity with the restoration under func-
tion, cold and warm stimuli, and a gentle air stream (on a
scale from 0 to 10).
• marginal discoloration and integrity
• secondary caries
• fracture
• vitality test
• retention
• interproximal contacts
The null hypothesis was that the self-curing mode does
not affect postoperative sensitivity.
RESULTS
The results of postoperative sensitivities are summarized in
Table 1. All 53 teeth were evaluated at baseline, and after 2
weeks and 6 months. At baseline, 3 patients showed pre-op-
erative sensitivity on 5 teeth. Ten cases of postoperative sen-
sitivity were observed at the 2-week recall, but only 3 after
6 months. At the 2-week recall, the postoperative sensitivi-
ty increased from 0 to 6 in one case immediately after lut-
ing the restoration (after the anesthetic wore off) but
dropped to score 3 after 6 months. In 7 cases showing an
increase in postoperative sensitivity after 2 weeks, the hy-
persensitivity disappeared completely after 6 months. In
two cases, a residual postoperative sensitivity of score 2 re-
mained after 6 months. No adverse events/effects oc-
curred. All other parameters showed alpha scores (Table 2).
DISCUSSION
Ceramic crowns can be considered a safe type of restoration,
and are reported to last longer than any other esthetic indi-
rect restoration,15 although many factors influence success,
such as the kind of ceramic, luting agent, and extension of
the lesion. Notwithstanding the restoration material, debond-
ing and thus microleakage at the gingival margins – particu-
larly if located below the cementoenamel junction – cannot
be completely prevented.1,8 All these factors are related to
three subjects: patient, dentist, and material.11
In order to control for any additional source of variation be-
sides the patient-related variability, one and the same oper-
ator placed all the restorations in this clinical trial. Inclusion
and exclusion criteria were followed in order to obtain the
Ethics Committee’s approval. The occurrence of postopera-

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Ferrari et al
tive sensitivity was found in around 19% of the restorations,
with an average score of 1.9. Only in one case of ten was the
postoperative sensitivity relatively high (score 6), while in
other cases, the sensitivity was not spontaneous. However,
at the 6-month recall, the score dropped from 6 (strong) to
3 (mild). This observation is in agreement with a study that
reported hypersensitivity to be the most common postoper-
ative complication.17
The accurate fitting of the crown is another aspect that is
worth mentioning, even though this property was not explic-
itly assessed in this paper. A good fitting of the ceramic
restoration can prevent postoperative sensitivity and pulp
complications. In several studies, it had been reported12,19
that the marginal wear of a composite luting cement can un-
dermine the mechanical support. To prevent excessive mar-
ginal wear, it is therefore mandatory to have the narrowest
possible gap between the cavity preparation and ceramic
restoration. Optimal fit (ranging from 50 to 100 μm) is pre-
ferred,8 particularly if the margins extend below the cemen-
toenamel junction.7,9
A proper adhesive-cement material combination is es-
sential for avoiding postoperative sensitivity. Other self-acti-
vated bonding systems are available on the market and have
been clinically tested.5,14 All of them are usually both self-ac-
tivated and light cured in order to guarantee complete poly-
merization of the bonding layer at the surface (where the
bonding agent can be reached by light) and in deeper areas
where light cannot penetrate to the adhesive layer.
The dual-curing resin cements are used in combination
with the proprietary bonding systems. Accordingly, with the
limits of this study, the mixture of XP BOND with SCA in com-
bination with chemically curing Calibra showed clinically ac-
ceptable levels of postoperative sensitivity at the 2-week
and 6-month recalls. These findings will be reevaluated dur-
ing next recalls at 12 months, and 2 and 3 years.
The utilization of a correct bonding technique is manda-
tory to achieve good clinical results in ceramic inlay luting.9
In direct resin restorations, the bonding agent is routinely
light cured prior to the insertion of the composite. In ceram-
ic luting procedures, pre-curing of the adhesive resin may
make restoration seating more difficult. Also in this regard,
the use of a self-curing bonding agent is advantageous. In
the present study, a self-curing cement was chosen for lut-
ing the restorations. The self-curing cements are able to
achieve an adequate degree of conversion even at sites
where light curing may be hindered by the thickness of the
ceramic. The setting time of the resin cement can also be di-
rectly correlated to room temperature, glass plate, and
mouth temperature.
CONCLUSIONS
XP BOND used in self-curing mode showed in only one case
of 53 luted restorations a spontaneous postoperative sen-
sitivity of medium intensity after 2 weeks, which dropped to
a mild grade after 6 months, while all other 9 cases showed
a very low degree of sensitivity.
282
ACKNOWLEDGMENTS
This research was sponsored by Dentsply DeTrey, Konstanz, Germany.
REFERENCES
1. Alavi AA, Kianimanesh N. Microleakage of direct and indirect composite
restorations with three dentin bonding agents. Oper Dent 2002;27:19-24.
2. Bergman MA. The clinical performance of ceramic inlays: a review. Aust
Dent J 1999;44:157-168.
3. Dagostin A, Ferrari M. In vivo bonding mechanism of an experimental dual
cure enamel-dentin bonding system. Am J Dent 2001;14:105-108.
4. Davidson CL. Luting cement, the stronghold or the weak link in ceramic
restorations. Adv Engineer Mater 2001;3:763-767.
5. Fabianelli A, Goracci C, Bertelli E, Davidson CL, Ferrari M. A clinical trial of
Empress II Porcelain inlays luted to vital teeth with a self-light-curing ade-
sive system and a self-curing resin cement. J Adhes Dent 2006;8:427-431.
6. Ferrari M, Mason PN. Adaptability and microleakage of indirect resin in-
lays: an in vivo investigation. Quintessence Int 1993;24:861-865.
7. Ferrari M, Mason PN, Fabianelli A, Cagidiaco MC, Kugel G, Davidson CL. In-
fluence of tissue characteristics at margins on leakage of class II indirect
porcelain restorations. Am J Dent 1999;12:134-142.
8. Ferrari M, Dagostin A, Fabianelli A. Marginal integrity of ceramic inlays
luted with a self curing resin system. Dent Mater 2003;19:270-276.
9. Frankenberger R, Krämer N, Petschelt A. Technique sensitivity of dentin
bonding: effect of application mistakes on bond strength and marginal
adaptation. Oper Dent 2000;25:324-330.
10. Hahn P, Schaller HG, Hafner P, Hellwig E. Effect of different luting proce-
dures on the seating of ceramic inlays. J Oral Rehabil 2000;27:1-8.
11. Hickel R, Manhart J. Longevity of dental restorations in posterior teeth and
reasons for failure. J Adhes Dent 2001;3:45-64.
12. Krämer N, Frankenberger R, Pelka M, Petschelt A. IPS Empress inlays and
onlays after four years- a clinical study. J Dent 1999;28:325-331.
13. Krämer N, Lohbauer U, Frankenberger R. Adhesive luting of indirect
restorations. Am J Dent 2000;13:60-76.
14. Krämer N, Frankenberger R. Clinical performance of bonded leucite –rein-
forced glass ceramic inlays and onlays after eight years. Dent Mater
2005;21:262-271.
15. Lee IB, Um CM. Thermal analysis on the cure speed of dual cured resin ce-
ments under porcelain inlays. J Oral Rehabil 2001;28:186-197.
16. Manhart J, Scheibenbogen-Fuchsbrunner A, Chen HY, Hickel R. A 2-year
clinical study of composite and ceramic inlays. Clin Oral Invest 2000;
4:192-198.
17. Manhart J, Chen HY, Neuerer P, Scheibenbogen-Fuchsbrunner A, Hickel R.
Three-year clinical evaluation of composite and ceramic inlays. Am J Dent
2001;14:95-99.
18. Millediing P, Örtengren U, Karlsson S. Ceramic inlay systems: some clinical
aspect. J Oral Rehabil 1995;22:571-580.
19. Molin MK, Karlsson SL. A randomized 5-year clinical evaluation of 3 ce-
ramic inlay systems. Int J Prosthodont 2000;13:194-200.
20. Raffaelli O, Cagidiaco MC, Goracci C, Ferrari M. XP BOND in self-curing
mode used for luting porcelain restorations. Part A: microtensile test. J
Adhes Dent 2007;9:275-278.
Clinical relevance: The results of this 6-month study re-
veal good clinical performance of XP BOND in self-curing
mode.
The Journal of Adhesive Dentistry
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