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Original Article

Self etching adhesive on intact enamel

Abstract
Background and Objective: to analyze the poor performance
of self-etch adhesives on intact enamel. Materials and
Methods: labial surfaces of 20 caries free permanent upper
central and lateral incisors were cleaned, sectioned of
their roots. All specimens were mounted on acrylic block
and divided randomly into two groups. In one group
the application of self-etch adhesive was carried as per
manufacturers instructions, composite cylinders were built,
whereas in the other group, 37% phosphoric acid was applied
before the application of self-etching adhesives. Then the resin
tags were analyzed using the scanning electron microscope.
Results: showed that when phosphoric acid was used,
there was significant increase in the depth of penetration of
resin tags. Conclusion: the results indicate that out of both
treatment groups, pre-etching the intact enamel with 37%
phosphoric acid resulted in the formation of longer resin tags
and higher depth of penetration of resin tags of the Clearfil
SE bond, which might have resulted in attaining higher bond
strength of the Clearfil SE bond to intact enamel.

Key words
Permanent maxillary incisors, phosphoric acid, pre-etching,
resin tag, self-etch adhesives, shear bond strength

Introduction
The introduction of enamel bonding leads to an
increasing demand for restorative and nonrestorative
esthetic treatments have transformed the practice of
operative dentistry.
The introduction of reliable[1] adhesive restorative
materials have substantially reduced the need for
extensive tooth preparations since the introduction
of acid etching by Buonocore in 1955. Although the
bond strengths of adhesive systems were satisfactory,
simplified adhesive systems were developed in order
to reduce the number of steps during the bonding
procedures.

Devarasa GM, Subba Reddy VV, Chaitra NL1

Department of Pedodontics and Preventive Dentistry, College

of Dental Sciences, Davangere, Karnataka, 1Department of
Pedodontics and Preventive Dentistry, Kothiwal Dental College
and Research centre, Kanth Road, Moradabad, Uttar Pradesh,
India
Correspondence:
Dr. G. M. Devarasa, Senior Lecturer, Department of
Pedodontics and Preventive Dentistry, College of Dental
Sciences, Pavilion Road, Davangere-577004, Karnataka, India.
E-mail: devrasgm@gmail.com
Access this article online
Quick Response Code:

Website:
www.jisppd.com
DOI:
10.4103/0970-4388.99987
PMID:
***

The first simplification was the fifth generation of bonding

agents, systems in which the primer and the adhesive were
mixed together and supplied as a single system.
Two systems even simpler to use were developed, one
consisting of an acidic primer and a bonding resin is
referred to as a sixth-generation adhesive and another
in which the etchant, primer, and adhesive are combined
into one single delivery system marketed as seventh
generation of adhesive systems.
Though the self-etching primers have been reported
to produce high bond strength to dentin, only limited
evidence exists reporting that self-etching primers can
be used for bonding composites to intact enamel.
The scanning electron microscopy helps us in the
assessment of bonding efficacy of the bonding agents
by examining the resin tag penetration depth.

Materials and Methods

A total of 20 teeth were divided into two groups of 10

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Devarasa, et al.: Pre etch before self etch?

samples each. The samples were cleaned and scaled using

ultrasonic scaling unit, the roots were sectioned and the
crowns were stored in distilled water. Routine prophylactic
procedure was carried out with rubber cup and aqueous
slurry of pumice for all the teeth before they were treated.

U analysis was used for groupwise comparisons.

Samples were mounted horizontally on acrylic resin

blocks. Teeth were mounted by keeping the labial
surface exposed.

This in vitro study was carried out to evaluate and

compare the resin tags of self-etch adhesives formed
on intact enamel with and without pre etching with
37% phosphoric acid.

Bonding agent was used as per manufacturers

instructions
Clearfil SE
Primer was applied on to the enamel surface and left
for 15 s, followed by gentle air drying; application of
adhesive and left for 10 s, followed by gentle air drying
and light curing for 10 s.

Bonding protocol foreach group

Group A: Self-etch adhesive was applied over intact
labial enamel as per manufacturers instructions.
Group B: Labial enamel was etched with 35%
phosphoric acid as per manufacturers instructions.
Self-etch adhesive was then used as like group A.
For group A and B, 1 mm thick layer of composite was
placed over the bonded enamel surface and cured for
40 s using Halogen light curing unit (3M ESPE) and
the specimens were store in deionized distilled water
at 37C for 24 h.

Resin tag analysis

The resin tag analysis was done using the scanning
electron microscope. The specimens from group A and B
were used for resin tag analysis.[Figure 1] The Crowns
were sectioned longitudinally in a labiolingual direction to
a thickness of 1 mm, using a hard tissue microtome. All
specimens were cleaned in distilled water with ultrasonic
agitation for 30 min and gently air dried. They were fixed
to SEM stubs, gold sputtered [Figure 2] for 10 min and
the resin enamel interface of the specimens were examined
under the SEM machine at an optical zoom of 2000 for
the evaluation of resin tags.[Figures 3,4]

Statistical analysis
Intergroup comparisons of the results of resin tags
were analyzed by MannWhitney U test. The mean
values (E*) were calculated for each group. The level
of significance for all the tests was chosen as P < 0.001
Results were expressed as mean SD. Mann Whitney
134

The P value was calculated for statistical significance.

Results (Resin Tags)

The samples after completing the bonding procedures

were sectioned using hard-tissue microtome, gold
sputtered, and examined under the scanning electron
microscope.
The resin tag analysis was done by measuring the depth
of the penetration of the resin tags into the enamel in
micrometers.
Table 1 shows the values of the different samples
of the group A and B regarding their range, mean,
median values of the resin tag penetration depths in
the micrometer.
Group A: The range of depth of the penetration of the
resin tags into the enamel in micrometers in group A
was 0-8.14 mm with a median depth of penetration of
4.07 mm with a mean of 3.67 mm.
Group B: the range of depth of the penetration of the
resin tags into the enamel in micrometers in group B
was 9.3-27.9 mm with a median depth of penetration
of 18.13 mm with a mean of 16.9 mm.
Table 2 shows the comparison of the two groups
regarding their Mean SD of the resin tag penetration
depths in micrometer.
The Mean SD of group A is 3.67 2.85 mm
The Mean SD of group B is 16.9 5.48 mm

Inter group comparisons

At the end of treatment the improvement in resin tag
penetration depth of self-etch adhesive on intact enamel
on pretreatment with 37% phosphoric acid was 95.4%.
The results showed that Group A demonstrated lower
resin tag penetration depths than Group B exhibiting
statistically significant difference with P value of
<0.001 [Table 2].

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Devarasa, et al.: Pre etch before self etch?

Table 1: Range, mean and median of resin tag penetration depths in micrometer of group A and B
Study Group (n = 10)

Range (micrometer)

Mean (micrometer)

Median (micrometer)

SD

0-8.14
9.3-27.9

3.67
16.90

4.07
18.13

2.85
5.48

Group A
Group B

Table 2: Mean and standard deviation of resin tag penetration

depths in micrometer of group A and B
Study group
(n = 10)

Mean SD

Z* Value

Significance

Group A
Group B

3.67 2.85
16.90 5.48

3.75

P < 0.001 Highly Significant

*Mann Whitney U test

Discussion
The enamel bonding potency of self-etch adhesives
over intact enamel is highly questioned mainly due
to its decreased efficacy in creating a definitive etch
pattern.
A bonding agent for giving better bond strength
on a dental substrate has to form a uniform wellpenetrating resin tags within the dental substrate.
Bonding to the intact surface of enamel is important
to prevent marginal leakage, and provide maximum
bond strength. In most studies investigators flattened
enamel surfaces using silicon carbide prior to
application of adhesives. So an in vitro study was
conducted to evaluate the resin tag formation of selfetch adhesives over intact enamel with and without
pre-etching with 37% phosphoric acid.
In this study, the investigations were carried out
on intact enamel that is very important for certain
procedures. The results of this study suggested that
adequate bonding to intact enamel with self-etch
adhesives alone cannot be achieved and will require
additional phosphoric acid etching for 15 s at a
concentration of 37% is used.
The intact enamel surface is hyperminerlized and
contains more fluoride than ground enamel. It is
reported that after teeth eruption, changes occur in the
outermost enamel. Saturated calcium phosphate might
hyper mineralize the enamel, and the fluoride ions might
convert the hydroxyapatite into fluorapatite. Thick
prismless enamel layer may prevent the permeation
of self-etching primers and bonding agents and thus
leaving some areas partially unetched, which may result
in formation of shorter and poorly defined resin tags.
Phosphoric acid etching removes the outermost enamel
and there by resulting in formation of longer resin tags
and there by increasing the bond strength.[2]

The aggressive etching effect of phosphoric acid on the

enamel surface overcomes the difficulty of conditioning
of intact or unprepared surfaces. The formation of a deep
etching pattern leads to similar bond strength, when the
adhesives are applied in both enamel surfaces.[3]
Self-etching systems contain acidic monomers based
on esters from phosphoric acid, carboxylic acid, or
their derivatives. Their etching efficacy and bonding
formation depends on the type of acidic monomer, pH of
adhesive solution, etching time, and application method.
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 agent.[4]
Marina Di Francescantonio reported that the pH
values of all self-etching systems were higher than
phosphoric acid. In general, the demineralization
effects of these systems are proportional to the
acidity of the acidic primers or self-etching adhesive
solutions. The self-etching primers are less aggressive
than phosphoric acid etchants, and do not form a
proper and defined acid etching pattern and the
conditioning effects are also reduced in intact enamel
surfaces, except for the Tyrian SPE primer, which
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 acid. 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 resin. These morphological features
of the resin-enamel bonds are different from that
formed with the etch and rinse adhesive systems.
This thin hybridized complex of resin formed in
enamel, 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 surfaces. Optibond
Solo Plus SE and One-Up Bond F systems performed
better on prepared enamel than on unprepared enamel.

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Devarasa, et al.: Pre etch before self etch?

Although Optibond Solo Plus SE primer presents low

pH (1.5), it did not bond to unprepared enamel, leading
to pretesting debonding in all specimens.[4]
For One-Up Bond F, SEM analysis of treated enamel
surfaces with the adhesive solution revealed an
extremely mild etching pattern, regardless of the
surface preparation. 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 us 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 selfetching adhesive to form a defined etching pattern for
infiltration of adhesive resin.[4]
The removal of superficial, aprismatic layer, by wetgrinding with 600-grit SiC paper improves the etching
effects. As the morphological structure and composition
of the intact peripheral surface of the enamel is
different from that of the middle enamel layer, these
differences can be favorable for etching effects in the
subenamel surface.
For Optibond Solo Plus SE and One-Up Bond F
systems, the enamel surface preparation resulted in
higher bond strength. Enamel preparation using 600grit SiC paper is unlikely to affect resin enamel bond
strengths.[4]
Pashley and Tay reported that the efficacy of selfetching 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 curing.[3]
Self-etching primers contain acidic monomer and water,
which decalcifies the inorganic parts of a tooth but
generally its acidity is weak. The acidic portion of the
primer is neutralized by the calcium and phosphate ions
released during decalcification of enamel, and thereby
the decalcification process of enamel is ceased. SEM
analysis has revealed that phosphoric acid etching
prior to application of the self etch adhesives, created
a deeper etching pattern and thicker tag-like resin
penetration than priming alone.[5]
SEPs have demonstrated a shallower etch pattern.
136

This might be simply because of a poorer penetration

of the SEP into the enamel porosities or the result of
interference from mineral precipitates on the enamel
surface that mask the etch pattern. Because the acidic
primer is not rinsed off, phosphorous and calcium ions
released from the hydroxyapatite crystal dissolution
remain suspended in the primer solution. With the
SEPs, the ionic precipitate remains embedded in the
resin after polymerization.[6]
Kanemura et al. concluded stating that the phosphoric
acid etching produced good resin adhesion to ground
and intact enamel, whereas the self-etch adhesives
clearfil liner bond II, Tokuso mac bond II produced
good bonds on ground enamel, but had lower bond
strength on intact enamel. The causes were attributed
to the hypermineralized intact enamel with higher
fluoride content and a thick layer of the prismless
layer on intact enamel. It was also seen that the resin
tags were shorter, poorly defined, and structurally
incomplete. Phosphoric acid etching removes the
outermost enamel layer and creates microirregularities
and thereby results in good penetration of the resin
etched intact enamel.[2]
Miguez PA study concluded saying that acid etching
prior to application of self-etching primer clearfil
SE bond, produced higher bond strength to enamel
than self-etching priming only. The self-etch primer
caused less demineralization of enamel compared
to the total etch systems. The shallower pattern of
demineralization is due to difficulty in penetration of
the primer into enamel and due to the precipitation of
minerals on enamel that might modify the depth of
demineralization.[7]
Perdigao reported that, Single Bond, the total-etch
adhesive, resulted in statistically higher microtensile
bond strength than any of the other adhesives
regardless of the enamel preparation. All self-etching
adhesives resulted in higher microtensile bond strength
when enamel was roughened than when enamel was
left unprepared. The field-emission scanning electron
microscope revealed a deep interprismatic etching
pattern for the total-etch adhesive, whereas the selfetching systems resulted in an etching pattern ranging
from absent to moderate.[8]
Marina Rotta concluded that all self-etching adhesives
showed lower uTBS values than those obtained in
phosphoric acid groups. Lower bond strength was
mainly attributed to the low acidity of self-etch

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Devarasa, et al.: Pre etch before self etch?

Figure 1: Labilolingual crossections For SEM

Figure 2: SEM Stubs and gold sputtered samples

Figure 3: Resin tags of self-etch adhesive without pre etching

Figure 4: Resin tags of self-etch adhesive with pre etching

less than the reference value observed with phosphoric

acid.[10]

Figure 5: Resin tag penetration depth

adhesives and less distinct etch pattern exhibited

when the enamel was conditioned with self-etching
adhesive. CSE exhibited the mildest etching pattern.
All self-etching adhesives applied after phosphoric
acid exhibited a more retentive etching pattern. It was
concluded that the bond strength values of low-pH selfetching adhesives can be improved by the adjunctive
use of phosphoric acid or replacement of the bonding
resin.[9]
Nasr stated that the demineralizing capacity of a
product depends on such factors as its pH (for strong
acids) or pKa (for weaker acids), its chelating ability, or
the solubility of its calcium salts and of the duration
of application. The strongest demineralizations are yet

Pisol Senawongse compared three commercially

available adhesive materials single bond (total etch),
Clearfil SE Bond (two step self etch), One-Up Bond
(one step self-etch) for their microshear bond strength
on intact and ground enamel. The results showed that
the two self-etching bonding agents showed lower
bond strength than the total etching system on intact
enamel, where as there was no significant differences in
the bond strength on ground enamel. The resin tags in
the single bond group revealed abundant longer resin
tags on both intact and ground enamel. In the case of
self-etch adhesives, short resin tags were seen in case
of ground enamel, whereas on intact enamel, the short
resin tags were rarely seen.[11]
Further studies testing these materials in vivo are
warranted to determine whether the amount of bonding
is the same as the in vitro study, is clinically relevant.

Conclusion
Within the limitations of this study conducted and the
results obtained, it can be concluded that

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Devarasa, et al.: Pre etch before self etch?

Out of both treatment groups, pre etching the intact

enamel with 37% phosphoric acid resulted in longer
resin tags (higher depth of penetration of resin tags)
and this can be the reason of low bond strength of self
etch adhesives on intact enamel.

6.
7.
8.

References
9.
1.
2.
3.
4.

5.

Roberson TM, Heymann HO, Swift EJ. Fundamentals of dental

bonding: Sturdevents Art and Science of Operative Dentistry.
Mosby 5th ed. 2006. p. 243-79.
Kanemura N, Sano H, Tagami J. Tensile bond strength to and
SEM evaluation of ground and intact enamel surfaces. J Dent
1999;27:523-30.
Pashley DH, Tay FR. Aggressiveness of contemporary selfetching adhesives. Part 2: Etching effects on unground enamel.
Dent Mater 2001;17:430-44.
di Francescantonio M, de Oliveira MT, Shinohara MS,
Ambrosano GMB, Giannini M. Bond strength evaluation of
self-etch and total-etch adhesive systems on intact and ground
human enamel. Braz J Oral Sci 2007;6:1462-6.
Torii Y, Itou K, Nishitani Y, Ishikawa K, Suzuki K. Effect of
phosphoric acid etching prior to self etching primer application
on adhesion of resin composite to enamel and dentin. Am J Dent
2002;15:305-8.

10.
11.

Cal-Neto JP, Miguel JA. Scanning electron microscopy evaluation

of the bonding mechanism of a self-etching primer on enamel.
Angle Orthod 2006;76:132-6.
Miguez PA, Castro PS, Nunes MF, Walter R, Pereira PN. Effect
of acid-etching on the enamel bond of two self-etching systems.
J Adhes Dent 2003;5:107-12.
Perdigo J, Geraldeli S. Bonding characteristics of self-etching
adhesives to intact versus prepared enamel. J Esthet Restor
Dent 2003;15:32-41.
Rotta M, Bresciani P, Moura SK, Grande RH, Hilgert LA,
Baratieri LN, et al. Effects of phosphoric acid pretreatment and
substitution of bonding resin on bonding effectiveness of self
etching systems to enamel. J Adhes Dent 2007;9:537-46.
Nasr K, Sharrock P, Grgoire G. Release of aqueous calcium and
phosphate from human dental enamel following administration of
self-etching adhesives. J Biomater Sci Polym Ed 2005;16:745-59.
Senawongse P, Sattabanasuk V, Shimada Y, Otsuki M, Tagami J.
Bond strength of current adhesives systems on intact and ground
enamel. J Esthet Restor Dent 2004;16:107-15.

How to cite this article: Devarasa GM, Subba Reddy VV, Chaitra
NL. Self etching adhesive on intact enamel. J Indian Soc Pedod
Prev Dent 2012;30:133-8.
Source of Support: Nil, Conflict of Interest: None declared.

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