A Comparison of the Tensile Bond Strengths of Composite Resins to Longitudinal
and Transverse Sections of Enamel Prisms in Human Teeth
T. MUNECHIKA, K. SUZUKI*, M. NISHIYAMA, M. OHASHI, and K. HORIEt
Department of Dental Materials, Nihon University School of Dentistry, 1-8-13, Surugadai, Chiyodaku, Tokyo; *Okayama University School of
Dentistry, 2-5-1, Shikatacho, Okayamashi, Okayama; and tNihon University School of Dentistry at Matsudo, 870-1, Sakaecho, Nishi-2,
Matsudoshi, Chiba, Japan
The tensile bond strengths of composite resins to transverse and
longitudinal sections of enamel prisms etched with phosphoric
acid were examined. The tensile bond strengths were 18-19 MPa to
the transverse and 10-11 MPa to the longitudinal sections and thus
were influenced by the nature of the enamel crystal planes. These
facts suggest that composite resin restorations will have a longer
life span if the enamel walls are given marginal forms to produce
transverse rather than longitudinal sections of enamel prisms.
J Dent Res 63(8):1079-1082, August, 1984
Introduction.
In previous studies, composite materials showed fairly high
bond strengths to etched human enamel (Rock, 1974;
Munechika et al., 1980; Beech and Jalaly, 198 1; Munechika
et al., 198 1; Munechika, 1983) and to human dentin when
used in combination with bonding agents or coupling
agents of several kinds of functional methacrylate mono-
mers (Suzuki et al., 1979; Suzuki et al., 1980; Bowen et al.,
1982; Munechika, 1983; Munechika et al., 1983). However,
composite restorations presently require the acid etch
technique with phosphoric acid to provide adequate bond
strength to enamel.
In vitro, the concentrations of phosphoric acid solution,
etching time, etched surface structure (Silverstone, 1974;
Munechika et al., 1980; Munechika et al., 1981), and bond
strengths of the composite materials (Rock, 1974; Mun-
echika et al., 1980; Beech and Jalaly, 1981; Munechika
et al., 1981) have been investigated on transverse sections
of enamel prisms, but in vivo, longitudinal sections of
enamel prisms are usually exposed when the cavity walls
are filled with composite materials.
Although resin tag formation (Crawford and Whittaker,
1977) has been studied, the bond strengths of composite
materials with the etched longitudinal sections of enamel
have not been investigated. A comparison of bond strengths
of composite materials to the longitudinal and transverse
sections of enamel prisms is necessary to determine the
influence of polymerization shrinkage forces on composite
materials in a cavity (Bowen et al., 1983) and the effects
of the marginal form of the cavity (Buonocore et al.,
1973; Galan et al., 1976).
In this study, the tensile bond strengths of composite
materials to longitudinal and transverse sections of enamel
prisms etched with phosphoric acid were investigated.
Materials and methods.
Preparation of test specimens. - Freshly extracted,
sound, human pre-molars were used. For the longitudinal
sections of enamel prisms, the crown was cut in a bucco-
lingual direction, and for the transverse sections of enamel
Received for publication January 18, 1984
Accepted for publication April 4, 1984
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prisms, the buccal surface was ground flat on a polishing
machine under a continuous flow of water. Both types of
surfaces were given a final polish with JIS # 1000 sandpaper.
These polished surfaces were dried with compressed air
immediately before use, etched with 40% phosphoric acid
solution for from ten to 180 sec, and then washed in run-
ning water and dried with compressed air. Oblong areas
measuring 1.2 x 3.0 mm on the etched enamel surface were
masked off with PVC self-adhesive tape, and the experi-
mental cavity for filling was then made by placing a poly-
ethylene ring on that. To one exposed surface was applied
the mixed bonding agent of Clearfil Bond System-F §
according to the manufacturer's recommendations, and the
mixed composite resin was immediately placed on it. To
another exposed surface was applied the bonding agent for
ultraviolet light-polymerized resins composed of N,O-
dimethacryloxy tyrosine (DMTY) (Suzuki et al., 1979)
and 2-hydroxy ethyl methacrylate (HEMA).¶ I nmediately
afterward, the composite resin [Bis-GMA (Bowen, 1962;
Suzuki et al., 1979) monomer, diluted by triethylene glycol
dimethacrylate° containing approximately 65% silica glass
particulate filler], of the ultraviolet light-polymerized type,
was placed on it. Following this, the resin was exposed to
ultraviolet light for polymerization with Duralux UV-300 '
for 120 sec (Munechika, 1983). After polymerization, the
polyethylene ring was removed from the specimens, and
they were stored in 370C water for 24 hr and then tested.
Measurement of tensile bond strengths. -On the speci-
mens, a brass cap attachment was fixed on top of the com-
posite resin, according to the method employed by Suzuki
et al. (1979). Tensile bond strengths were measured with an
Instron Universal Tensile Machine equipped with the
tensile adhesive test apparatus using a tensile speed of 2.0
mm/min.
For each measurement a minimum of 12 specimens was
tested.
Results.
The tensile bond strengths of Clearfil Bond System-F to
different sections of enamel prisms are shown in Fig. 1. The
tensile bond strengths to the enamel prisms sectioned trans-
versely (a) increased as the etching time was lengthened, to
a maximum of approximately 19 MPa, with an etching time
of 60 sec, but decreased with further etching time.
The tensile bond strengths to the enamel prisms sec-
tioned longitudinally (b) increased slightly as the etching
time was lengthened, to a maximum of 11 MPa, with an
etching time of 60 sec, but decreased slightly with further
etching time.
§ Kuraray Co., Ltd., Okayama, Japan
¶ Tokyo Kasei Kogyo Co., Ltd., Tokyo, Japan
"Sin-Nakamura Chemical Co., Ltd., Wakayama, Japan
oKulzer Co., Ltd., Bad Hamburg, West Germany
*Minebea Co., Ltd., Tokyo, Japan
1079
1080 MUNECHIKA ETAL.
25
(a)
~20
t15
"0T
0 J
0 £ f. . IL
10 30 60 90 120
etching time (sec.)
Fig. 1 - Effects of etching time with 40% phosphoric acid on tensile bond strengths of composite resins to (a) transverse and (b) longitudinal
sections of enamel prisms. The standard deviation: H-.
*to convert MPa to kilograms of force per square centimeter, kg/cm2, divide by 0.098044.
The tensile bond strengths of Clearfil Bond System-F
and of a UV-polymerized composite resin, using trial
bonding agent DMTY-HEMA, to different sections of
enamel prisms are shown in Fig. 2. The tensile bond strengths
were approximately 18 MPa to the transverse sections
and approximately 11 MPa to the longitudinal sections
etched with 40% phosphoric acid for 60 sec. By Stu-
dent's t test, statistically significant differences in bond
strengths at the 95% confidence level were found between
the transverse and longitudinal sections (Figs. 1 and 2),
but not between the two types of bonding agents (Fig. 2).
SEM photographs of fractured enamel and composite
surfaces after measurement of tensile bond strengths are
shown in Figs. 3 and 4. SEM views obtained indicated that,
in the transverse sections (Fig. 3), the composite resins
used with either of the bonding agents (Clearfil or DMTY-
HEMA) fractured cohesively, and pieces of composite resin
were left on the enamel. In the longitudinal sections (Fig.
4), the enamel, with both bonding agents, fractured co-
hesively, and pieces of enamel were left on the composite
resin.
Discussion.
For investigations of acid-etching of enamel, the labial
surfaces of upper central incisors are mostly used. The
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J Dent Res August 1984
(b)
. . A.
180 10 30 60 90 126 180
enamel surface is composed of transverse sections of
enamel prisms and produces a honeycombed structure with
acid-etching (Munechika et al., 1980; Munechika et al.,
1981).
Recently, it has been reported that the honeycombed
structure varies with type and concentration of acid and
with etching time, and that these influence the bond
strengths of the composite resins (Silverstone, 1 974;
Munechika et al., 1980; Munechika et al., 1981). The
tensile bond strengths of 18-19 MPa between composite
resin and transversely sectioned, etched enamel surfaces
exceeded the cohesion of the composite resin, and, as a
result, the composite resins fractured cohesively. Tensile
bond strengths to longitudinal sections of etched enamel
were unrelated to the length of etching time or the type
of bonding agent used. The values of 10-11 MPa were lower
than those with the transverse sections, but the enamel
still fractured cohesively. The values for tensile bond
strength are similar to the tensile strength of enamel itself
(10.3 MPa) (Bowen and Rodriguez, 1962). The poly-
merization shrinkage forces (5.2-7.6 MPa) (Bowen et aL.,
1983) in a composite resin bonded to longitudinally sec-
tioned enamel may affect the enamel walls. This poly-
merization shrinkage force accounts for from 60-80% of the
tensile bond strength of composite resins to longitudinal
sections of enamel.
Vol. 63 No, 8 TENSILE BOND STRENGTHS OF COMPOSITE RESINS 1 081

25 transverse
It has been conjectured that the enamel walls in cavities
are fractured by thermal stresses (Hassan et al., 1 981 ) or by
_~ longitudinal external forces such as biting forces, resulting in marginal
leakage. Our study indicates that the bond strength be-
tween composite resin and enamel improves when the
enamel walls of the cavities are contoured to give transverse
sections of the enamel prisms.
I In practice, this suggests that cavity margins should be
bevelled and not finished as butt joints.
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