Braz J Oral Sci. October-December 2007 - Vol.

6 - Number 23

Bond strength evaluation of self-etch

and total-etch adhesive systems on
intact and ground human enamel
Marina Di Francescantonio1
Marcelo Tavares de Oliveira2
Mirela Sanae Shinohara3
Glucia Maria Bovi Ambrosano4
Marcelo Giannini5
1

DDS, Graduate student (Master degree),

Department of Restorative Dentistry
2
DDS, MSc, Graduate student (Doctor degree),
Department of Restorative Dentistry
3
DDS, MSc, PhD, Assistant Professor, School of
Dentistry, State University of Amazonas, Manaus,
AM, Brazil
4
DDS, MSc, PhD, Professor, Department of
Social Dentistry
5
DDS, MSc, PhD, Associate Professor,
Department of Restorative Dentistry
Piracicaba Dental School, State University of
Campinas, Piracicaba, SP, Brazil

Received for publication: October 10, 2007

Accepted: December 20, 2007

Correspondence to:
Marcelo Giannini
Department of Restorative Dentistry
Operative Dentistry Division
Piracicaba Dental School State University of
Campinas
Av. Limeira, 901 Piracicaba/SP Brazil CP 52
CEP: 13414-903
Telephone: +55 19 21065338
Fax: +55 19 21065218
E-mail: giannini@fop.unicamp.br

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Abstract
The aim of this study was to evaluate the bond strength of adhesive
systems to intact and ground enamel. Enamel blocks from buccal and
lingual surfaces of third molars were used for bonding procedures.
Intact or ground (600-grit SiC paper) enamel surfaces were bonded
using two etch&rinse adhesives (Prime&Bond 2.1 and Single Bond),
three self-etching primer systems (Optibond Solo Plus SE; Tyrian
SPE/One-Step Plus and UniFil Bond) or two self-etching adhesives
(One-Up Bond F and Xeno III). A 6-mm composite crown was built
on the bonded surfaces and samples were stored for 24 hs at 37oC.
Samples were sectioned into 0.9-mm-thick slabs, each slab trimmed
to a cross-sectional area of 0.8 mm2 and specimens loaded to failure at
a crosshead speed of 0.5 mm/min, using a universal testing machine.
Microtensile bond strength data (n=6) were analyzed using KruskalWallis and Dunn tests. Differences in bond strength between intact
and ground surfaces were not significant for both etch&rinse
adhesives, Tyrian SPE/One-Step Plus, UniFil Bond and Xeno III
systems. The enamel surface preparation resulted in higher bond
strength for Optibond Solo Plus SE and One-Up Bond F systems.
Enamel preparation using 600-grit SiC paper is unlikely to affect
resin-enamel bond strengths.
Keywords:
dental enamel, dentin-bonding agents, tensile strength.

Braz J Oral Sci. 6(23):1462-1466

Bond strength evaluation of self-etch and total-etch adhesive systems on intact and ground human enamel

Introduction
Although phosphoric acid has been intensely used to etch
the dental substrates (enamel and dentin) for bonding, selfetching adhesives are consider alternative methods to prepare
the tooth for restorative procedures. Self-etching adhesive
systems were developed in attempt to simplify the clinical use
of dental adhesives, because they do not require separated
phosphoric acid etching, water-rinsing or superficial moist
controlling steps. The self-etching primers and adhesives are
composed of aqueous solutions of acidic functional monomers
and methacrylate components, with a pH relatively higher than
that of phosphoric acid etchants1.
While the adhesion to dentin produced by self-etching
adhesives has been considered effective 2, studies are in
disagreement regarding the efficacy of conditioning and
monomer infiltrations on enamel3-6. Morphological analyses
of enamel surface treated with self-etching primers have
showed not very demineralized surfaces and other areas that
were predominantly unetched, which could impair the monomer
infiltrations and hybridization process7-10.
To improve the bonding of self-etching systems to enamel, it
has been recommended, surface pre-treatments, increase in
acidic monomer concentration, increase of etching time as
well as different application methods 3,8,11-12. Moreover, the
removal of superficial, aprismatic layer could facilitate the
etching and the infiltration of adhesive monomers7,13-14, forming
a strong and durable bonding. The purpose of this in vitro
study was to evaluate the bond strength of self-etching
adhesive systems and conventional systems (etch & rinse
adhesives) to intact and ground enamel. The null hypothesis
was that bond strength is not influenced by the characteristics

of the enamel surface (intact and ground) regardless of the

type of adhesive system used.
Materials and Methods
Forty-two extracted, caries-free erupted human third molars
were used in this study according to protocols approved by
the institutional review board of the Piracicaba School of
Dentistry University of Campinas (069/2003). Teeth were
obtained by patients from 19 to 25 years old and stored in
physiological saline solution with 0.1% thymol for no longer
than 3 months.
Tooth roots were severed and the crowns were longitudinally
sectioned (mesio-distally direction) into two-halves, using a
diamond blade (Isomet, Buehler Ltd., Lake Bluff, IL, USA)
under water cooling. Eighty-four dental fragments were
obtained (6 mm in length X 5 mm in width X 1.0 mm in thickness).
A buccal or a lingual flat enamel surface of each fragment was
chosen and selected for conditioning treatments and bonding
procedures. All specimens were randomly assigned to fourteen
groups (n = 6), according to surface treatment of enamel
(grounded and intact) and type of adhesive system (selfetching and etch & rinse systems). The dental fragments
from the grounded surface groups had their enamel surface
abraded with a #600-grit SiC paper on a polishing machine
(APL-4, Arotec S.A. Ind. Com., Cotia, SP, Brazil) under water
cooling for 15 seconds.
Seven adhesive systems: two 2-step etch & rinse single
bottle adhesives (Single Bond and Prime&Bond 2.1), three 2step self-etching primer systems (OptiBond Solo Plus SE;
Tyrian SPE/One-Step Plus and Unifil Bond) and two one-step
self-etching systems (One-Up Bond F and Xeno III) were

Table 1 - Compositions of adhesive systems used in this study.

Adhesive Systems

Composition

pH

One-Up Bond F
(self-etching
adhesive)

Bonding A: Water, methyl methacrylate, HEMA, coumarin dye, metacryloyloxyalkyl acid phosphate, MAC10.
Bonding B: multifuntional methacrylic monomer, fluoraluminosilicate glass, photoinitiator (arylborate
catalyst)

2.6

okuyama Dental Corp,

Taitou-ku, Tokyo,
Japan

OptiBond Solo Plus

SE
(self-primer)

Primer: Ethyl alcohol, water, alkyl dimethacrylate resins, stabilizers, activators.

Adhesive resin: uncured methacrylate ester monomers, photo-initiators, stabilizers.

1.5

Kerr,
Orange, CA,
USA

Prime&Bond 2.1
(etch & rinse)

Etchant: 34%phosphoric acid.

Adhesive: PENTA dimethacrylate resins UDMA cetylamine hydrofluoride acetone

2.4

Dentsply DeTrey,
Konstanz Germany

Single Bond
(etch & rinse)
Tyrian SPE/One-Step
Plus
(self- primer)

Etchant: 35%phosphoric acid.

Adhesive: Bis-GMA, HEMA, ethanol, water, UDMA, bisphenol A glycerolate, polyalkenoic acid copolymer,
dimethacrylate canphorquinone

4.3

Manufacturer

3M ESPE,
St. Paul, MN,
USA

Primer: 2-acrylamido-2-methyl propanesulfonic acid, bis (2-(methacryloyloxy) ethyl) phosphate, ethanol.

Adhesive: Biphenyl dimethacrylate, hydroxyethyl methacrylate, acetone, glass frit.

0.5

sco Inc., Schuamburg, IL,

USA

UniFil Bond
(self-primer)

Primer: HEMA, 4-MET, ethanol, water.

Adhesive resin : UDMA,HEMA, TEGDMA, silanated colloidal silica.

2.2

GC Corp.,
Itabashi-ku, Tokyo,
Japan

Xeno III
(self-etching
adhesive)

Liquid A: HEMA, purified water, ethanol, butylated hydroxy toluene, highly dispersed silicon dioxide.
Liquid B: phosphoric acid functionalised polymethacrylate resins, di- and polyfunctionalised methacrylate
resins, butylated hidroxy toluene, camphorquinone, 4-dimethylamino-ethyl-benzoate.

1.4

Dentsply DeTrey,
Konstanz,
Germany

Bis-GMA = bisphenol-glycidyl-methacrylate; HEMA = 2-hydroxyethylmethacrylate; PAA = polyalkenoic acid copolymer; MAC-10 =

methacryloxyundecane dicarboxylic acid; TEGDMA = triethylene glycol dimethacrylate; 4-MET = 4-methacryloxyethyl trimellitate anhydride;
UDMA = urethane dimethacrylate; PENTA: dipentaerythritol penta-acrylate monophosphate.

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Braz J Oral Sci. 6(23):1462-1466

Bond strength evaluation of self-etch and total-etch adhesive systems on intact and ground human enamel

Table 2 - Median values (range) of bond strength for experimental groups.

Enamel

Adhesive System

Unground

One-Up Bond F

Ground

5.8 (5.6 - 9.2) B b

16.4 (10.2 20.1) A ab

OptiBond Solo Plus SE

0.0 (0.0 - 0.0) B c

12.8 (5.0 13,0) A b

Prime&Bond 2.1

23.7 (16.7 - 23.4) A a

24.3 (13.4 28.6) A a

Single Bond

19.8 (11.2 - 23.6) A ab

18.3 (12.9 22.5) A ab

Tyrian SPE/One-Step Plus

21.1 (17.2 - 28.2) A a

20.8 (12.8 23.9) A ab

UniFil Bond

16.0 (8.7 17.3) A ab

17.2 (9.6 18.9) A ab

Xeno III

25.0 (11.1 30.6) A a

21.5 (10.9 28.4) A ab

Medians followed by different letters (lower case column, upper case row) differ among them by Kruskal-Wallis and Dunn tests.

evaluated (Table 1). Adhesive systems were applied according

to the manufacturers instructions. Resin composite build-ups
were constructed incrementally on the adhesive-bonded
surfaces of enamel in 3, 2-mm thick layers using a hybrid resin
composite (Clearfil APX; Kuraray Medical Inc, Kurashiki,
Japan). Each layer was light-cured for 40 s (670 mW/cm2) using
a light-curing unit (XL 3000; 3M ESPE, St. Paul, MN, USA).
After 24 hours of water storage, restored fragments were
sectioned into 0.9 mm thick slabs with a diamond blade (Isomet
1000; Buehler Ltd, Lake Bluff, IL, USA). For each fragment
sectioned, 2 slabs were selected and prepared for micro-tensile
bond strength testing. Each slab was ground at the bonded
interface and along both sides with a fine diamond rotary
cutting instrument (#8835KR.314.012; Brasseler, Lemgo,
Germany) under water irrigation to produce an hour-glass
shaped specimen. This reduced the cross-sectional area of
the specimen necks (0.7 0.7 mm) to approximately 0.8 mm2
for micro-tensile strength testing. Each specimen was fixed to
the grips of a micro-tensile testing device with cyanoacrylate
adhesive (Zapit; DVA, Corona, CA, USA) and tested in tension
in a testing machine (4411, Instron Corp., Canton, MA, USA)
at 0.5 mm/minute until failure. After testing, specimens were
carefully removed from the device with a scalpel blade (BD,
Franklin Lakes, NJ, USA). The cross-sectional area at the site
of fracture was measured to the nearest 0.01 mm with a digital
caliper (Starret 727-6/150; Starret, Itu, SP, Brazil) and used to
calculate test results in units of stress (MPa). Means of the
two specimens (hour-glass shaped) were calculated for each
restored tooth fragment. Microtensile bond strength data were
analyzed statistically by Kruskal-Wallis and Dunn tests.
Results
Table 2 shows the median values of tensile bond strength for
the adhesive systems applied to intact and ground enamel.
For Optibond Solo Plus SE and One-Up Bond F systems, the
grounding of enamel surface before adhesive application
improved the bond strength. When applied them on intact
enamel surfaces, low bond strengths were found for One-Up
Bond F and pre-testing debonding occurred for specimens

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restored with Optibond Solo Plus SE.

For most adhesive systems (Prime&Bond 2.1, Single Bond,
Tyrian SPE/One-Step Plus, UniFil Bond and Xeno III), the
enamel surface preparation did not increase the bond strength.
In the cases of bonding to grounded enamel, the adhesive
systems produced similar bond strengths; however OptiBond
Solo Plus SE had lower bond strength than Prime&Bond 2.1.
Discussion
Although some studies suggested to abraded the enamel
surface before application of moderate or mild two-step selfetching primers or single-step, all-in-one adhesives7,10,13, the
results of this study indicated that only two of them had theirs
bond strengths increased by surface preparation with #600grit SiC paper. Thus, the null hypothesis was only partially
confirmed because two self-etching adhesive systems tested
were influenced by the characteristics of the enamel surface.
The two etch & rinse, one-bottle adhesives (Prime&Bond 2.1
and Single Bond), which are used after conditioning with
phosphoric acid, were not affect by abrading or not the enamel
surface. The grounded or the unprepared enamel surfaces
treated with phosphoric acids result in an etching pattern,
which consist of the formation of a porous surface with
exposed enamel crystallites and dissolution of both inter and
intraprismatic areas. The aggressive etching effect of
phosphoric acid on enamel surface overcomes the difficulty
of conditioning of intact or unprepared surfaces. The formation
of a deep etching pattern6,10,15 lead to similar bond strength
when the adhesives are applied in both enamel surfaces.
Self-etching systems contain acidic monomers based on esters
from phosphoric acid, carboxylic acid or derivatives6-7,12-13. Their
etching efficacy and bonding formation depends on type of
acidic monomer, pH of adhesive solution, etching time and
application method6,8,16. Acidic monomers are responsible for
etching the dental substrates, whereas methacrylate
components, such as HEMA, are available for monomer
infiltration and polymerization of the bonding agent3-4,12. Selfetching systems can be classified as strong, moderate and
mild, depending on their etching aggressiveness or acid

Braz J Oral Sci. 6(23):1462-1466

Bond strength evaluation of self-etch and total-etch adhesive systems on intact and ground human enamel

dissociation constants (pKa values)2,6. In this study, it was

selected a strong system (Tyrian SPE primer), two moderates
(OptiBond Solo Plus SE and Xeno III) and two milds (Unifil
Bond and One-Up Bond F).
Studies have shown that most of the self-etching adhesives
did not etch enamel as deeply as the phosphoric acid etchants
did and the shallow etching pattern could compromise the
bonding to enamel3,13,17. Pashley and Tay6 reported that the
efficacy of self-etching primers in intact enamel does not
depend solely upon their etching aggressiveness, but on
monomeric composition of each material. It is also possible
that the low enamel bond strengths might be caused by the
high amount of unpolymerized acidic monomers remaining
after curing4. Thus, no correlation among degree of primer
aggressiveness, enamel etching pattern and bond strength to
intact enamel has been established for self-etching adhesives18.
The pH values of all self-etching systems tested were higher
than phosphoric acid. In general, the demineralization effects
of these systems are proportional to the acidity of the acidicprimers or self-etching adhesive solutions. The self-etching
primers are less aggressive than phosphoric acid etchants, do
not form a proper and defined acid etching pattern3,7,13-14 and
the conditioning effects are also reduced in intact enamel
surfaces, except for Tyrian SPE self-etching primer10.
The Tyrian SPE primer is considered a strong self-etching
adhesive with a very low pH (0.5). The etching pattern formed
on both ground and intact enamel surfaces is similar to that
promoted by phosphoric acid10. Moderate self-etch systems
include Optibond Solo Plus SE and Xeno III adhesives with
pH 1.4 and 1.5, respectively, while Unifil Bond (pH 2.2) and
One-Up Bond F (pH 2.6) systems are considered mild. The
bonding mechanism of these self-etching systems to enamel
is based on nanoretentive interlocking between crystallites
and adhesive resin18-19. These morphological features of the
resin-enamel bonds are different from that formed with the
etch&rinse adhesive systems18-20. This thin hybridized complex
of resin formed in enamel and produced by self-etchings
without the usual micrometer-size resin tags can be responsible
for lower bond strengths presented by some self-etching
systems and the questionable effectiveness of this type of
dental adhesives on enamel surfaces9,21-22.
Optibond Solo Plus SE and One-Up Bond F systems performed
better on prepared enamel than on unprepared enamel.
Although Optibond Solo Plus SE primer presents low pH (1.5),
it did not bond to unprepared enamel, leading to pre-testing
debonding in all specimens. Moreover, Shinohara et al.10 did
not observed proper conditioning effects promoted by the
acidic primer on intact enamel surfaces, which could
compromise the adhesion to enamel, as observed in this study.
However, Xeno III and Unifil Bond present similar and higher
pH than Optibond Solo Plus SE, respectively, and were not
affected by the mode of enamel surface preparation. Thus,
other factors, such as, monomer infiltration, polymeric network

formation and degree of conversion could also influence on

the results of bond strength.
For One-Up Bond F, SEM analysis of treated enamel surfaces
with adhesive solution revealed an extremely mild etching
pattern, regardless of the surface preparation 10,13,15. This
probably occurred due to the very mild pH (2.6) of the system,
which would not provide adequate demineralization for
infiltration of monomers. This pattern helps to explain the bond
strength results, which were lower when compared to the
ground surface. The higher bond strengths to the SiC-prepared
surface can be attributed to the roughness of the surface that
facilitates the activity of the self-etching adhesive to form a
defined etching pattern for infiltration of adhesive resin.
The removal of superficial, aprismatic layer by wet-grinding
with 600-grit SiC paper improves the etching effects7,10,13. As
the morphological structure and composition of the intact
peripheral surface of the enamel is different from that of the
middle enamel layer23, these differences can be favorable for
etching effects in sub-enamel surface. Since in clinical
situations the enamel is usually prepared with dental drills
prior to application of the adhesive system, the concerns about
effectiveness of self-etching adhesives can be reduced.
In conclusion, most of the self-etching systems and the two
etch & rinse adhesives showed the similar bond strength
values for grounded or intact enamel surfaces. For Optibond
Solo Plus SE and One-Up Bond F systems, the enamel surface
preparation resulted in higher bond strength Enamel
preparation using 600-grit SiC paper is unlikely to affect resinenamel bond strengths.
Acknowledgement
This study was supported by grants 01/13034-3 from FAPESP
and by grants from Capes, Brazil.
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