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UTS Giannini

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Dental Materials (2004) 20, 322–329

http://intl.elsevierhealth.com/journals/dema

Ultimate tensile strength of tooth structures


Marcelo Gianninia,*, Carlos José Soaresb, Ricardo Marins de Carvalhoc

a
Department of Restorative Dentistry, Piracicaba School of Dentistry, University of Campinas, Av. Limeira,
901, Piracicaba, SP, Brazil
b
Department of Operative Dentistry, School of Dentistry, University of Uberlândia, Uberlândia, MG, Brazil
c
Department of Operative Dentistry, Endodontics and Dental Materials, Bauru School of Dentistry,
University of São Paulo, Bauru, SP, Brazil

Received 23 October 2002; received in revised form 20 March 2003; accepted 28 April 2003

KEYWORDS Summary Objective. This study determined the ultimate tensile strength (UTS) of
Tensile strength; enamel (E), dentin (D) and dentin –enamel junction (DEJ) using the microtensile
Enamel; Dentin; Dentin– technique. It was hypothesized that the UTS of dental structures varies according to
enamel junction location and nature.
Methods. Intact occlusal enamel surfaces from extracted human third molars were
etched with 37% phosphoric acid and bonded with a one-bottle adhesive system. The
bonded occlusal surfaces received a resin composite build-up and teeth were serially,
vertically sectioned into several 0.7 mm thick slabs. Each slab was then trimmed to a
dumbbell-shaped specimen with irrigated diamond burs to reduce the cross-sectional
area to approximately 0.5 mm2 at E, D or DEJ. E was tested according to its prismatic
orientation (parallel, EP; and transversally, ET) and D as function of depth (superficial,
DS; middle, DM and deep, DD). Specimens were tested in tension in an Instron testing
machine at 0.5 mm/min. Results were analyzed by one-way ANOVA and Duncan’s
Multiple Range test.
Results. UTS mean values ðN ¼ 20Þ were, MPa (SD): DEJ, 46.9 (13.7)b; EP, 42.1
(11.9)b; ET, 11.5 (4.7)d; DS, 61.6 (16.2)a; DM, 48.7 (16.6)b and DD, 33.9 (7.9)c. Enamel
stressed transversally to its prismatic orientation was significantly weaker ðp , 0:05Þ:
Dentin depth significantly affected its UTS ðp , 0:05Þ: DEJ presented UTS that was
similar to EP and DM ðp . 0:05Þ:
Significance. The UTS of dental structures varies according to its nature and
location.
Q 2003 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Introduction the tooth includes highly mineralized tissues that


present physical properties based on their compo-
The tooth is the only mineralized organ that is sition and micro morphology.1 The anatomical
located partially internal and partially external crowns of teeth are covered by dental enamel,
to the body. To minimize wear during function, which is the hardest tissue in the body, and is
composed of 92 – 96% of inorganic matter, 1 –2% of
*Corresponding author. Tel.: þ 55-194305340; fax: þ 55- organic material and 3 –4% of water by weight.1
194305218. Most of the inorganic matter is hydroxyapatite that
E-mail address: [email protected] is contained in the basic structural unit of enamel,

0109-5641/$ 30.00 Q 2003 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.
doi:10.1016/S0109-5641(03)00110-6
Ultimate tensile strength of tooth structures 323

the rod or prism.2 Enamel hardness is attributed to may still induce such cohesive failures in the
its high mineral content3 and the brittle property is substrate with this technique.21,28 Therefore, to
due to its high elastic modulus and low tensile facilitate the interpretation of the microtensile
strength.4 Clinically, enamel cracks and fracture bond strength data when failures occur within the
can occur despite enamel being a very strong substrate, it is important to determine the UTS of
substrate. Studies have shown that enamel is the substrate using the same microtensile method.
anisotropic and its mechanical properties may be The purpose of this study was to determine the
dependent on the type and direction of the stress UTS of enamel, dentin and DEJ as a function of their
applied, as well as the prismatic orientation.5 – 8 orientation and location. Enamel was tested
Between enamel and dentin, a biological inter- according to its prismatic orientation, transversally
face may dissipate stresses inhibiting further crack or parallel; the occlusal DEJ was tested; and dentin
propagation.9,10 The dentin– enamel junction (DEJ) was tested as function of depth: superficial, middle
has a high fracture toughness and, along with the and deep. In addition, fractured surfaces were
more resilient underlying dentin, supports the examined under a scanning electron microscope
integrity of enamel by preventing its fracture during (SEM) to determine the failure patterns. Two
function.11 hypotheses were tested: the first hypothesis was
Dentin is a hydrated biological composite com- that the apparent UTS of the DEJ is closer to that of
posed of 70% inorganic material, 18% organic matrix enamel than to dentin. The second hypotheses was
and 12% water (wt%), with properties and structural that deep dentin is weaker than superficial dentin.
components that vary with location.12 The collagen
phase of intertubular dentin contributes to a lower
modulus of elasticity than enamel, while the lower
mineral content is associated with a decrease in Materials and methods
dentin microhardness as compared with enamel.13
The structural composition of dentin includes Twenty sound human third molars that were
oriented tubules surrounded by a highly mineralized refrigerated in a solution of 0.05% thymol for no
cuff of peritubular dentin and an intertubular longer than one month after extraction were
matrix consisting of type I collagen fibrils cleaned of gross debris and placed in distilled
reinforced with apatite.14,15 The relative contri- water for 24 h before beginning the experiment.
bution of tubules, peritubular and intertubular The teeth used in this study were obtained under
dentin varies significantly in composition with the protocol (75/99) that was analyzed and
location.16 These differences in composition are approved by the Ethical Committee in Research at
thought to have profound effects in its tensile the Piracicaba Dental School/UNICAMP, Piracicaba,
strength.17 SP, Brazil.
Due to improvements in the ability of adhesive Intact occlusal enamel surface was etched with
systems to bond to dental tissues, there has been an 37% phosphoric acid for 30 s, rinsed and bonded
increase in the frequency of cohesive failures of with single bond (3M ESPE, St Paul, MN, USA). A
dentin during bond strength testing. This precludes resin composite block (6 mm high) was incremen-
the determination of the real interfacial bond tally built up in three layers with TPH Spectrum
strength and has been shown to occur more resin composite (Dentsply Caulk, Milford, DE, USA)
frequently when conventional shear or tensile to form an extension of the crown to facilitate
methods are used.18 – 20 further slicing and testing (Fig. 1a). Each increment
Since its introduction in 1994, the microtensile was light-cured for 20 s and the specimens were
technique5 has proven to be a very useful tool to stored in water at 37 8C for 24 h.
measure not only the bond strength of adhesive The roots were removed approximately 3 mm
materials to dental tissues, but also to determine below the cemento –enamel junction using a dia-
the ultimate tensile strength (UTS) of both mond disk (KG Sorensen, Barueri, SP, Brazil)
materials and tooth substrates.5,17,18,22 – 26 Major mounted in a low-speed handpiece. The remaining
advantages of the microtensile technique include crown was then serially, vertically sectioned in a
improved stress distribution during adhesion test- buccal– lingual direction (Fig. 1b) to obtain several
ing18,27 and the ability to perform the test in very slices of approximately 0.7 mm thick (Fig. 1c). Six
small specimens.18 Although a reduced number of slices of each tooth were selected and randomly
cohesive failures within the substrate is usually assigned into six groups ðn ¼ 20Þ: The slices were
reported when the microtensile technique is used to trimmed to an ‘hourglass’-shape with a superfine
assess the bond strength of resin materials to dental diamond bur under air– water irrigation (Fig. 1d)
tissues,18,21 high-performance adhesive systems to reduce the DEJ (Fig. 1e), enamel or dentin to
324 M. Giannini et al.

Figure 1 Schematic representation of specimen preparation. (g) Enamel parallel to the prism orientation; (f) enamel
stressed perpendicular to enamel prisms. (e) DEJ stressed parallel to enamel prisms; (j) deep dentin was tested; (i)
orientation for testing middle dentin parallel to the long axis of the tubules; (h) superficial dentin was tested.

a cross-sectional area of 0.5 mm 2 . DEJ and (DSM 940A, Zeiss, Oberkochen, Germany). Repre-
enamel specimens were obtained from the internal sentative areas of the tested sites were photo-
slope of the buccal cusps. Enamel was trimmed in graphed at 2000 £ and 5000 £ magnifications.
such a way that permitted the testing by
applying the load in an orientation either transver-
sal to its prismatic orientation (Fig. 1f) or parallel
to its prismatic orientation (Fig. 1g). Dentin Results
was trimmed as a function of depth: trimming
was done 1 mm (superficial), 2 mm (middle) or The analysis of variance revealed that there were
3 mm (deep) below the occlusal DEJ (Figs. 1h –j, significant differences among the UTS of the dental
respectively). substrates ðp , 0:05Þ: Table 1 shows the average
Each specimen was fixed to the grips of the UTS of the substrates. Superficial dentin showed the
microtensile testing device with cyanoacrylate glue highest mean tensile strength (61.64 MPa, p , 0:05)
(Zapit, Dental Vent. Am., Corona, CA, USA) and of all the substrates. The lowest values were
tested in tension at 0.5 mm/min in a universal
testing machine (4411, Instron Co., Canton, MA,
USA) until failure. After fracture, the specimen was Table 1 Ultimate tensile strength (MPa) of tooth structures.
removed from the testing apparatus and the cross- Tooth structure Mean (SD)
sectioned area at the site of fracture measured with
a digital caliper (727, Starrett Ind. Com. Ltda., Itu, Superficial dentin 61.6 (16.3)a
SP, Brazil) to the nearest 0.01 mm. Mean tensile Middle dentin 48.7 (16.7)b
strength values were expressed in MPa and data Deep dentin 33.9 (8.0)c
Dentin–enamel junction 46.9 (13.7)b
were analyzed by one-way ANOVA, followed by
Parallel enamel 42.2 (12.0)b
Duncan’s Multiple Range test at a ¼ 0:05: Transversal enamel 11.5 (4.7)d
The specimens were allowed to air-dry over-
Means indicated by different letters are significantly different
night, sputter-coated with gold (MED 010, Balzers,
at p , 0:05; N ¼ 20 per group.
Balzer, Leichtenstein) and examined under an SEM
Ultimate tensile strength of tooth structures 325

observed for enamel when tested transversally to


its prismatic orientation (11.49 MPa, p , 0:05).
Dentin depth significantly influenced the strength
of dentin as it became weaker closer to the pulp
ðp , 0:05Þ: Enamel was significantly stronger when
tested parallel to its prismatic orientation ðp ,
0:05Þ: The strength of the DEJ was similar to that of
middle dentin and enamel when tested parallel to
its prismatic orientation ðp . 0:05Þ:
Representative SEM micrographs of the frac-
tured site of the specimens are shown in Figs.
2 – 6. All dentin specimens were fractured across
the trimmed area. For superficial dentin, a larger
area of solid dentin and low tubule density are
noted (Fig. 2). In contrast, a relative increase in
the area occupied by tubules and a reduced area
of solid dentin are observed in deeper dentin
(Fig. 3). In general, fractures did not occur in a
sharp, single plane along the intertubular and
peritubular dentin. Fractures across the peritub- Figure 3 Fractured site in deep dentin. Tubules are
ular dentin occurred either above or below the larger in diameter and occupy a relatively larger area of
plane of fracture of the intertubular dentin the surface. A similar fracture pattern as for superficial
(Figs. 2 and 3). and middle (not shown) dentin was observed. The plane of
fracture changes abruptly from intertubular to peritubular
SEM observation showed that most DEJ speci-
dentin (arrows). Original magnification £ 10,000.
mens actually fractured along the weaker neighbor-
ing enamel, thus, intact areas of DEJ can be noted individual prisms (Fig. 5). A characteristic
(Fig. 4). When enamel was stressed parallel to its fracture pattern was observed for enamel tested
prismatic orientation, fractures occurred preferen- transversally to the orientation of prisms. Fractures
tially obliquely to the long axis of the prisms, occurred preferentially along the interprismatic
leaving them prominent on the surface. Cone-like
ends were generally seen at the fractured site of

Figure 4 Fracture site near the dentin – enamel junc-


tion. The DEJ is intact as the fracture occurred in the
Figure 2 Fractured site in superficial dentin. Intertub- neighboring enamel. At the enamel side (E), typical
p
ular dentin occupies most of the area ( ). An abrupt oblique fractures of enamel prisms can be noted as they
change in the plane of fracture was observed at the were stressed parallel to their orientation (arrows).
boundaries between intertubular and peritubular dentin Dentin (D) adjacent to the DEJ. Original magnification
(arrows). Original magnification £10,000. £ 5000.
326 M. Giannini et al.

Discussion

Bond strength testing methods are designed to


determine the interfacial strength between the
bonded substrates. However, in such testing, the
applied load cannot be exclusively concentrated at
the interface, but it is rather distributed and
modified along the bonded substrates, depending
on the composition of the substrates and the
geometry of the testing assembly.19,20 Therefore,
the intrinsic strength of the bonded substrates can
act as a modifier of the resultant apparent bond
strength value.28 – 30 When testing resin bond
strength to dentin using conventional shear testing,
cohesive failures within the substrate have been
reported to occur in the range of 20 –30 MPa.18
Because the intrinsic cohesive strength of dentin
has been reported to be much higher (ca. 50 –
130 MPa),11,17,22,31,32 fractures below those values
Figure 5 Fractured site of enamel tested parallel to its are generally confusing and attributed to other
prismatic orientation. An irregular surface consisting of
factors related to the testing method.19,20,29
cone-shaped structures (arrows) was observed. As the
fracture did not occur in a single plane, these structures
Gwinnett 33 demonstrated that the cohesive
appeared protruding from the surface. Original magnifi- strength of dentin was about 30 – 35 MPa when
cation £ 5000. tested in specimens with a similar geometry to
that used with the shear bond strength method,
substance and parallel to the long axis of the prisms. indicating a more realistic value for that specific
Oblique fractures across the prisms could be noted testing method.
at sites where the prism changes its orientation Over the last 5 years, there have been an
(Fig. 6). increasing number of studies using the microtensile
technique to evaluate the bond strength of
adhesive materials to dental tissues. This method
tends to decrease the number of pure cohesive
failures within the substrates compared to conven-
tional testing techniques.18,34 However, since
cohesive failures of dentin still occur, it is import-
ant to determine the strength of the dental
structures when tested using the similar microten-
sile technique.
Most of the tooth structure is comprised of
dentin. The tubule density and the area occupied by
solid dentin vary with distance from the pulp
chamber to the DEJ.35 – 37 Several studies have
investigated the relationship between
microstructure and the mechanical properties of
dentin.1,17,22,23,31,38,39 Results indicated that cohe-
sive strength of dentin varies significantly and is
dependent on intra-tooth location.6,24,32,38,40 In
this study, statistically significant differences
were found in the UTS of dentin as function of
depth. Our results confirm that dentin becomes
Figure 6 Fractured site of enamel tested transversally
to its prismatic orientation. Fracture plane occurred
weaker closer to the pulp than near the DEJ, as
preferentially along the interprismatic substance. When- previously demonstrated by others.17,24,32,38,39
ever prisms changed their orientation, oblique fractures These results support the second hypothesis that
of the prisms were noted (arrows). Original magnification deep dentin is weaker than superficial dentin. It is
£ 5000. evident that the empty lumina of the tubules do not
Ultimate tensile strength of tooth structures 327

contribute to the strength of dentin, therefore, the i.e. around or between prisms, which behave as
relative larger area of solid dentin in superficial integral units and are less likely to cleave under
rather than in middle and deep dentin explains the tension.6 – 8 A significantly lower load was able to
findings. Our values are within the same range as fracture enamel when it was loaded in a direction
those previously reported for specimens originating perpendicular to the orientation of the prisms
from the same regions in dentin and tested under (Table 1). This is similar to the results of other
similar methods.17,24 Sano et al.22 reported higher studies.7,25,28 In that situation, the weaker inter-
UTS values for dentin when the tensile force was prismatic substance is also aligned perpendicular to
directed perpendicular to the tubule orientation. the load and rapidly propagates the tension across
Further, their specimens had a smaller cross- the specimen causing it to fail under a lower
sectional area (ca. 0.25 mm2) and that is known to tension. In such a case, enamel prisms are separated
result in apparent higher values of either interfacial from one another along the interprismatic sub-
or cohesive strength of materials.17,21 Our speci- stance and only a few are obliquely cleaved. When
mens were tested with the load applied parallel to enamel is stressed parallel to its prismatic orien-
the orientation of the tubules. Apparently, dentin is tation, the tension concentrates on the stronger
stronger when the load is applied transversally to prismatic units and the fracture requires that all the
that orientation. 17 Since specimens for bond prisms be cleaved before catastrophic failure can
strength testing are generally prepared on a occur. This results in significantly higher UTS for
transversally flattened dentin surface, usually enamel when tested under this condition (Table 1).
located in superficial or middle dentin, our results Figs. 5 and 6 show the fracture pattern of both
indicate that bond strength values above 45 MPa orientations and are consistent with previous
may generate cohesive failures of dentin when reports.6,25 The mechanical behavior of enamel
using the microtensile technique. has profound relevance for clinical bonding pro-
The DEJ is a unique junctional zone between cedures.25 Depending on the location and treatment
highly mineralized tissues of different embryogenic of enamel margins in a cavity, factors such as the
origins, matrix composition and physical proper- presence of a bevel, contraction stresses generated
ties. SEM investigations of DEJ surfaces showed during the polymerization of the resin and the
that both enamel and dentin are scalloped in moment of finishing and polishing, enamel cracks
nature.41,42 None of the specimens tested in this may occur and ultimately compromise the clinical
study fractured solely along the DEJ. Fractures success of the restorative procedure.21,28,44,45
occurred more frequently in enamel and cracks Enamel butt joint margins at both occlusal and
always propagated following the orientation of the cervical areas are more likely subjected to stresses
prisms. Thus, the results support the first hypoth- produced by restorative procedures45 and the need
esis that the apparent UTS of the DEJ is closer to for placement of a bevel at such margins has been
enamel than to superficial dentin. It is interesting recently questioned.21,28
to note that the average UTS of the DEJ was not The results of this study indicate that the UTS of
significantly different from the UTS of enamel dentin, the DEJ and enamel vary widely. Addition-
when stressed parallel to its prismatic orientation ally, enamel showed an anisotropic behavior and
(Table 1). By the way we prepared our enamel dentin strength was influenced by intra-tooth
specimens, the orientation of the enamel prisms location. Perhaps deep dentin is weaker because
just below the DEJ was parallel to the enamel it has larger, more numerous tubules and that these
prisms (Fig. 1e). Similar fracture patterns and tubules might serve as sites for crack initiation.38
strength values were obtained by recent studies on The study provides data on the mechanical proper-
the physical properties of the DEJ.5,43 The lack of ties of such structures that were tested under
pure interfacial failure can be attributed to the conditions similar to those when using the micro-
complexity of DEJ structure and its ability tensile bond strength method. Such information
to modify crack propagation.5,8 It must be empha- may be useful for a better understanding and
sized that the ‘DEJ’ values do not represent interpretation of bond strength data obtained
the UTS of the DEJ, but that of nearby enamel. using microtensile method.
The toughness of the DEJ precluded attempts to
measure its UTS.
Previous studies on the physical properties of
enamel have considered it as a brittle structure with Conclusion
anisotropic behavior.2,6 – 8,25 Crack propagation
analysis usually demonstrates that enamel fractures The results of this study confirm that the UTS of
occur preferentially along the weakest path, tooth structures is dependent on intra-tooth
328 M. Giannini et al.

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