d e n t a l m a t e r i a l s 2 4 ( 2 0 0 8 ) 426–431

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Flexural strength and Weibull analysis of a microhybrid

and a nanofill composite evaluated by 3- and
4-point bending tests

Sinval A. Rodrigues Junior a,∗ , Jack L. Ferracane b , Álvaro Della Bona c

a Department of Operative Dentistry, Federal University of Pelotas, Pelotas, RS, Brazil
b Department of Biomaterials and Biomechanics, Oregon Health and Science University, Portland, OR, USA
c School of Dentistry, University of Passo Fundo, P.O. Box 611/613, Passo Fundo, RS 99001-970, Brazil

a r t i c l e i n f o a b s t r a c t

Article history: Objectives. The aim of the present study was to evaluate the flexural strength and the Weibull
Received 22 November 2006 modulus of a microhybrid and a nanofill composite by means of 3- and 4-point bending tests.
Received in revised form 7 May 2007 Methods. Thirty specimens of Filtek Z250TM (3M/ESPE) and Filtek SupremeTM (3M/ESPE) were
Accepted 15 May 2007 prepared for each test according to the ISO 4049/2000 specification. After 24 h in distilled
water at 37 ◦ C the specimens were submitted to 3- and 4-point bending tests using a univer-
sal testing machine DL2000 (EMIC) with a crosshead speed of 1 mm/min. Flexural strength
Keywords: data were calculated and submitted to Student’s t-test (˛ = 0.05) and Weibull statistics. The
Composite resin fractured surfaces were analyzed based on fractographic principles.
Nanofiller Results. The two composites had equivalent strength in both test methods. However, the
Flexural strength test designs significantly affected the flexural strength of the microhybrid and the nanofill
Weibull statistics composites. Weibull modulus (m) of SupremeTM was similar with both tests, while for
Fractography Z250TM , a higher m was observed with the 3-point bending test. Critical flaws were most
often associated with the specimen’s surface (up to 90%) and were characterized as surface
scratches/grooves, non-uniform distribution of phases, inclusions and voids.
Significance. Flexural strength as measured by the 3-point bending test is higher than by the
4-point bending test, due to the smaller flaw containing area involved in the former. Despite
the large difference in average filler size between the composites, the volume fraction of the
filler in both materials is similar, which was probably the reason for similar mean flexural
strength values and fracture behavior.
© 2007 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

1. Introduction composites contain a high percentage of inorganic reinforcing

Direct restorative composites experience considerable
mechanical challenge during function, especially those indi-
cated for posterior restorations. Thus, in order to withstand
the mechanical stress generated by the biting forces, these
filler [1].
A huge variation in the size, shape and constitution of filler
particles can be observed in the different commercial resin
composites, even for those of the same category or from the
same manufacturer [1]. Improvements in filler technology for

∗
Corresponding author at: School of Dentistry, Department of Operative Dentistry, Gonçalves Chaves Street, 457, Pelotas, RS 96015-560,
Brazil. Tel.: +55 53 32226690; fax: +55 53 32255581.
E-mail address: rodriguesjr2002@yahoo.com.br (S.A.R. Junior).
0109-5641/$ – see front matter © 2007 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.
doi:10.1016/j.dental.2007.05.013
 d e n t a l m a t e r i a l s 2 4 ( 2 0 0 8 ) 426–431
Fig. 1 – Test design of both, 3-point (A) and 4-point (B) bending tests.
composites increased the variety of options available and even
classifications of such materials have been suggested based on
the morphology of the filler particles [2].
Studies have shown the influence of the size and shape
of the filler particles on the mechanical properties of den-
tal composites [1–3]. These particle characteristics determine
what Braem et al. [4] called “maximum particle pack-
ing fraction”, which is the ratio of true particle volume
to the apparent volume occupied by the particles in the
composite. According to the authors, important mechani-
cal properties, such as Young’s modulus, depend upon this
ratio. Also, the presence of small spherical particles has
been related to a high percentage of filler in the com-
mercial composites, improving the mechanical properties
[2].
Nanotechnology has become a reality in different areas
of engineering with the development, through physical and
chemical methods, of materials and functional structures
containing particles within a size interval of 0.1–100 nm. It
is also one of the most noticeable advances in composite
filler technology, involving the incorporation of silica fillers
of nanometer size [5]. Nanofillers are found in microfill and
some hybrid composites that can be considered predecessors
of the newer nanoparticulate composites. A study evaluating
the mechanical properties of experimental composites with or
without nanofillers was carried out by Musanje and Ferracane
[6], who observed a positive effect of the presence of nanofiller
particles, expressed by an improvement in flexural strength,
surface hardness (H) and fracture toughness (Kc ).
Nanoparticulate composites bring the perspective of cre-
ating another category of universal resin composite that joins
the optical properties and the polishability required for ante-
rior restorations with the mechanical properties demanded
for posterior restorations [5,7,8]. However, relatively little
information about these new materials is available in the den-
tal literature.
Strength () is an important property for a restorative
material. It is dependent upon the material’s microstructure,
composition, testing method, environment and failure mech-
anisms [9]. Strength values are valuable when representing
information about the flaw population with potential to cause
the failure of a restoration or prosthesis, and thus, must be
interpreted within a context that involves the analysis of fail-
ure and structural reliability, rather than an isolated result
[9,10]. The presence of structural defects with potential to
become critical defects, such as microcracks, grains or inter-
nal voids depend upon the volume of the material structure
[11,12].
427
Measurement of the strength of composites is often per-
formed through flexural tests. The test indicated by the
International Standards Organization to evaluate the strength
of polymer-based restorative materials is the 3-point bend-
ing test (3PBT) [13]. This test employs bar-shaped specimens
that bend under compressive loading equally distant from the
lower supports, promoting tensile stresses in the lower sur-
faces that are more likely related to the fracture initiation
(Fig. 1A). The test configuration tends to confine the area sub-
mitted to the stress between the supporting rollers and the
loading rollers. The so-called 4-point bending test (4PBT) uses
the same bar-shaped specimens, but a different configuration
for load appliance based on two load cylinders over the upper
surface of the specimens (Fig. 1B) that tend to expose a higher
flaw containing area of the material to the stress when com-
pared to the 3PBT [14,15]. Therefore, it is expected that higher
strengths are measured with the three-point bending test.
Statistical parameters are commonly applied to data from
mechanical strength tests to determine the level of structural
reliability of the materials [16]. The Weibull modulus (m), or
shape parameter, describes the variation in the distribution
of strength values from different materials and also estab-
lishes a direct relationship with the size and distribution of
the defects present in a specific volume of material. In this
sense, high Weibull modulus indicates a smaller error range,
and potentially greater clinical reliability [16,17]. The charac-
teristic strength ( 0 ), or scale parameter, is also provided by
the Weibull statistics and represents the stress responsible
for 63.2% of the sample failures [10,12,15,17]. In addition, the
Weibull analysis can offer more clinically relevant parameters,
such as the 5% failure probability ( 0.05 ) [17].
The aim of the present study was to evaluate the flexural
strength of a microhybrid and a nanofill composite by means
of 3PBT and 4PBT, testing the hypothesis that the mean flexu-
ral strength values of both composites are higher for the 3PBT
than for the 4PBT. The structural reliability of the composites
with both tests was evaluated by means of Weibull statistics.
Fracture analysis was also performed in order to determine
and characterize the fracture initiation sites.
2. Materials and methods
2.1. Flexural strength tests
Thirty specimens of the composites Filtek Z250TM (batch
no. 5AG, shade D3, 3M/ESPE, St Paul, MN, USA) and Fil-
tek SupremeTM (batch no. 5AB, shade D2B, 3M/ESPE, St
428 d e n t a l m a t e r i a l s 2 4 ( 2 0 0 8 ) 426–431

Table 1 – Composition of the composites Filtek Z250TM and Filtek SupremeTM and curing times, according to the
manufacturer
Material Organic matrix Inorganic filler composition Shade Light curing
composition time (s)

Filtek Z250TM (Z2) Bis-GMA, UDMA and 60% in volume (range of D3 20

bis-EMA 0.19–3.3 ␮m)—zirconia and silica
Filtek SupremeTM (SU) Bis-GMA, bis-EMA, 59.5% in volume (clusters of D2B 20
UDMA and TEGDMA 0.6–1.4 ␮m—individual particle size of
5–20 nm)—zirconia and silica

Paul, MN, USA) (Table 1) were prepared for each test using
a bipartite stainless steel mold with internal dimensions
of 25 (±2 mm) × 2 (±0.1 mm) × 2 (±0.1 mm), according to ISO
4049/2000 specifications [13]. The mold was positioned over a
glass slide and a polyester strip and filled with one of the com-
posites, which was inserted in a single increment. Another
polyester strip was positioned and pressed against the restora-
tive material with a glass slide for removal of the excess before
polymerization. The specimens were irradiated on the top and
bottom surfaces, with five light exposures of 20 s, overlap-
ping the previously irradiated section with half the diameter
of the light guide, by a LED curing unit (LCU) (Radiie, serial
no. 39447, SDI, Victoria, Australia) with a power density of
500 mW/cm2 , measured with a hand radiometer Model 100
(batch no. 118568, Demetron Research Corp., Danbury, CT,
USA) before the procedure. The specimens were finished with
320 grit metallographic paper and stored in distilled water at
(37 ± 1) ◦ C for 24 h.
The specimen’s dimensions were measured with a digital
caliper (Mitutoyo Co., Kawasaki, Japan) before testing. The 3-
and 4-point bending loads were applied using a universal test-
ing machine DL2000 (EMIC, serial no. 092, Sao Jose dos Pinhais,
PR, Brazil) with a crosshead speed of 1 mm/min (Fig. 1). The
flexural strength () values were obtained from the 3PBT, in
MPa, based on the following formula:
where P is the maximum load (N), L the distance between the
supports (20 mm), w the width (2 mm) and b is the height of
the specimen (2 mm) [17].
2.2. Fracture analysis
The fractured surfaces of the specimens were sputter coated
with gold-palladium for 30 s in a Denton Vacuum Desk II
(serial no. 41878, Denton Vacuum Inc., NJ, USA) at a current
of 45 mA and a vacuum of 50 mTorr. They were observed in
light microscopy (LM) at 60× magnification (Stereomicroscope
Wild M5A, serial no. 245663, Leica Heerbrugg, Switzerland)
and scanning electron microscopy (SEM) (JXA 6400 Electron
Probe Microanalyzer, serial no. SM150041-174, Jeol, Ltd., Tokyo,
Japan).
2.3. Statistical analysis
Data obtained from the flexural tests were submitted to
Student’s t-test for differences between composites in each
flexural test and for the flexural test methods with the same
composite (˛ = 0.05). Weibull statistics were also carried out in
order to obtain the shape (m) and scale ( 0 ) parameters of both
composites.

3PL
= (1) 3. Results
2wb2
where P is the maximum load exerted on the specimen (N),
There was no significant difference between the two com-
L the distance between the supports (20 mm), w the width
posites evaluated, either for the 3PBT (p = 0.307) or the 4PBT
(2 mm) and b is the height of the specimen (2 mm).
(p = 0.275). However, a significantly higher flexural strength
The formula used for the 4-point flexural strength calcula-
with the 3PBT was observed for both, the microhybrid
tion was:
(p = 0.004) and the nanofill composites (p = 0.005), in compar-
PL ison with the 4PBT, confirming the hypothesis of the study
= (2)
wb2 (Table 2).

Table 2 – Mean flexural strength () in MPa and standard deviation (S.D.), number of specimens per group (n), Student’s
t-test grouping (˛ = 0.05), coefficient of variation, Weibull modulus (m) and standard error, 95% confidence interval of m,
characteristic strength ( 0 ) and standard error, 95% confidence interval of  0 , coefficient of correlation (r value), 5% failure
strength ( 0.05 ) and standard error
Group n  (S.D.) t-Student* CV (%) m (S.E.) 95% CI  0 (S.E.) 95% CI r  0.05 (S.E.)

3P-SU 30 149.4 (20.4) A, a 13.7 8.3 (1.0) 6.5–10.6 157.9 (3.7) 150.9–165.2 0.98 110.4 (6.4)
3P-Z2 30 154.0 (13.6) A, a 8.8 13.1 (1.5) 10.5–16.5 159.8 (2.3) 155.3–164.5 0.98 127.5 (4.5)
4P-SU 30 135.7 (15.3) B, b 11.2 9.7 (1.5) 7.1–13.0 142.5 (2.8) 137.1–148.1 0.99 104.8 (5.8)
4P-Z2 30 140.7 (19.9) B, b 14.1 7.6 (1.3) 5.5–10.5 149.5 (3.8) 142.3–157.0 0.99 100.9 (7.5)

∗
Different upper case letters indicate significant difference between composites in each flexural test and different miniscule letters indicate
significant difference between flexural test designs with each composite.
 d e n t a l m a t e r i a l s 2 4 ( 2 0 0 8 ) 426–431 429

Table 3 – Fracture analysis (in number of specimens (n) and the respective percentage)
Group Number of pieces Fracture origin

2 3 Surface flaw Internal flaw

n % n % n % n %

3P-SU 20 66.7 10 33.3 26 86.6 4 13.4

3P-Z2 18 60 12 40 27 90 3 10
4P-SU 9 30 21 70 29 96.6 1 3.4
4P-Z2 13 43.3 17 56.7 28 93.3 2 6.7

Corner defects identified in each group: 3P-SU = 5; 3P-Z2 = 6; 4P-SU = 6; 4P-Z2 = 7.

The characteristic strength ( 0 ) was lower in the 4-point test

Fig. 2 – Weibull cumulative failure curves of the flexural
strength of both, Filtek SupremeTM (SU) and Filtek Z-250TM
(Z2) with 3-point (3P) and 4-point (4P) bending tests.
for both, Z2 and SU.
All fractures initiated on the tensile side of the specimens.
For the specimens of the 3PBT, all the fractures occurred under
the applied load equidistant from both lower supports. How-
ever, an increased area of fracture initiation sites, all located
within the area of the load points, was observed for the 4PBT.
Surface defects represented the fracture initiation sites in
approximately 9 out of 10 specimens, regardless the type of
composite evaluated and the test method (Table 3). The critical
defects resulted from processing (inclusions and inhomoge-
neous distribution of the phases in the material) or handling
of the composite (surface voids and scratches), as shown in
Fig. 3A–F.

The cumulative probability of failure of the composites, 4. Discussion

expressed by means of the Weibull modulus (m), presented
similar values for 3P-SU, 4P-SU and 4P-Z2 (Table 2, Fig. 2). The Filler morphology and size are always factors of concern when
value of m for 3P-Z2 was significantly higher than the others. mechanical properties and fracture behavior of composite

Fig. 3 – Defects associated with fracture initiation: (A) surface defect attributed to material processing (Z2-4P—700X); (B)
surface void (Z2-4P—300X); (C) surface defect (arrow) connected to a internal pore (Z2-4P—300X); (D) corner defect
(Z2-3P—450X); (E) surface defect possibly caused by the inhomogeneous distribution of matrix and filler in the composite or
some other inclusion (SU-3P—300X); (F) internal defect with irregular shape, probably attributed to a cluster of pores
(Z2-4P—300X).
430 d e n t a l m a t e r i a l s 2 4 ( 2 0 0 8 ) 426–431
resins are evaluated, because they affect the filler volume frac-
tion [2]. In the present study, the flexural strength was not
affected by the differences of three orders of magnitude in
average filler size between the two composites (p = 0.307). This
is in accordance with other studies that showed no signifi-
cant difference in flexural strength between Filtek SupremeTM
(nanofill) and some microhybrid composites [5,8]. According
to Mitra et al. [5], a high filler loading was obtained in Fil-
tek SupremeTM due to the wide particle distribution and the
spherical shape of the filler particles, equaling physical and
mechanical properties of microhybrid composites, including
the flexural strength. The filler content of this composite is
composed of 20 nm non-aggregated silica particles and nan-
oclusters of 75 nm agglomerated particles that are reported to
reach a 0.6–1.4 ␮m size range that, in turn, corresponds to the
average size of the filler particles of Filtek Z250TM . In addition,
both composites contain spherical-shaped particles that have
been associated with reduced stress concentration as com-
pared with the sharp edges present in irregular-shaped filler
particles [1]. These factors in association with the similar filler
packing between the composites might have produced their
similar mechanical behavior.
The Weibull statistics is considered to be an accept-
able approach in engineering to evaluate the reliability of a
material or component. It provides a way of accessing the
dependability of the material, disclosing the probability of
failure at any selected level of stress. As a measure of the vari-
ability of strength in a material and its dependence on crack
size distribution, a higher m, even in association with slightly
lower mean fracture strength, is often preferable to a lower m
associated with a higher mean fracture strength [16]. A high
m could also be useful as an indicator of a more favorable test
design to evaluate and compare the strength of materials [18].
The overall Weibull modulus results confirmed the vari-
ability of strength of both composites with the different tests,
expressed by means of the standard deviation and the coef-
ficient of variability (Table 2 and Fig. 2). A significantly higher
m was shown for the microhybrid composite when tested by
3PBT. No significant difference, however, was found between
the tests for the nanofill composite. Similar results were found
by Jin et al. [18] when testing the flexural strength of ceram-
ics. The authors concluded that it is difficult to determine,
based on the Weibull modulus, the most suitable test design
for different materials.
Weibull statistics have been developed and used since the
1950s in the engineering community to determine equivalent
strengths that have been measured by different test con-
figurations. Weibull size scaling is routinely used to predict
strength for a 3PBT when strength is measured by a 4PBT, or
vice-versa. This is done by means of calculating “effective vol-
umes” or “effective areas” that are under stress, and is fairly
straightforward for the configurations of this study. Calcula-
tion of Weibull size scaling is done with the following formula:
 3 / 4 = (A4 /A3 )1/m , where  3 and  4 are the stresses measured
under 3- and 4-point configurations, A3 and A4 are the effective
areas of the associated configurations, and m is the Weibull
modulus. The effective area for 3PBT is (S/4)[(m + 2)/(m + 1)2 ]
and for 4PBT is (S/12)[(m + 2)(m + 3)/(m + 1)2 ], where S is the total
specimen surface within the load span and is the same for
both configurations, for the span lengths and specimen sizes
are the same [14]. Calculations predicted a 15% higher strength
for the 3-point configuration in comparison to the 4-point con-
figuration for either material. This is slightly higher than the
measured results (about 10%), but within experimental error.
The fracture behavior of the composites was also expressed
by  0 and  0.05 . Both parameters indicated a lower stress for
fracture of the composites when submitted to the 4PBT. This
might be explained by the fact that a higher volume (53.4%) is
exposed to the stress in the 4PBT comparing to the 3PBT (40%).
The macroscopic observation of the composite specimens
fractured by 4PBT disclosed fractures occurring in different
places along the tensile surface over distances between the
upper loading rollers, confirming also the wider volume of
material involved in this test. In contrast and as expected, the
specimens submitted to 3PBT fractured on the tensile surface
midway between the two supports. According to Zeng et al.
[11] the 3PBT submits only a very small area to the maximum
tensile stress, underestimating the flaws located far from the
loading rollers and tending to induce a fracture initiation site.
In this sense, although the 4PBT presented lower strength
values for both composites, it may represent a more reliable
approach as a measure of flexural strength of composites than
the 3PBT. In addition, it may provide a more realistic and ‘safe’
lower boundary for the resulting strength.
The analysis of the fractured surface using fractographic
principles is a well-established analytic tool to determine the
failure behavior of brittle materials. It is based on the principle
that the history of the fracture process is encoded on the frac-
tured surface of the material [12,19]. According to Le May and
Begnall [20], “investigations of structural failure by brittle frac-
ture should take into account, at least, two separate aspects:
(1) the point from which the fracture developed is relevant
in order to determine whether the fracture initiated from a
manufacturing effect, whether it experienced a prior fatigue
or stress corrosion that originated the crack that led to failure;
(2) it should indicate that, for whatever the defect present, the
load applied was enough for unstable fracture to occur”.
Characteristically, brittle materials, such as composites,
present a population of flaws of different sizes, geometries
and orientations. Fracture occurs when the load exceeds a
critical value for the propagation of the largest and most favor-
ably oriented flaw [10]. These flaws are induced by intrinsic
imperfections in the structure of the material, by processing or
by mechanical grinding and polishing, and might potentially
reduce the strength of the material [2,17,21].
The defects that led to the fracture initiation were iden-
tified as non-homogeneous distributions of organic and
inorganic phases, inclusions, cracks and voids. Both, the man-
ufacturing of the materials and the handling procedure might
generate these defects. In the present study, defects similar
to the flaw represented in Fig. 3A, presenting a smooth darker
area of matrix, were strongly associated with the initiation of
fracture.
Surface flaws were identified as the fracture initiation site
(critical flaw—c) for 86.6–96.6% of the specimens, independent
of the group (Table 3 and Fig. 3A–E). The low area exposed to
the maximum tensile stress in the bending test makes frac-
tures more likely to develop from the surface. In this sense,
bending specimens are considerably sensitive to surface or
edge damage during grinding or polishing [15]. Internal critical
 d e n t a l m a t e r i a l s 2 4 ( 2 0 0 8 ) 426–431
defects were rare and always associated with moderate to high
fracture strength. The internal irregular defects, like the one
presented in Fig. 3F, are more stress inducing than internal
spherical-shaped pores, requiring a lower load to propagate
the fracture.
The polymerization method employed, that was common
to both tests, also might have affected the fracture behav-
ior of the composites. According to Le May and Begnall [20],
fracture initiation and propagation depend on the total local
stress, which includes the externally applied load and the
residual stress of the specimen. This is of major importance,
because the production of 25 mm long bar-shaped specimens
requires an overlapped light activation procedure when using
an 11 mm diameter light guide, resulting in areas of the speci-
men that are exposed to twice the light [22,23]. Attempting to
avoid the effect of the inhomogeneous polymerization of the
specimens some authors have suggested the use of oven-LCUs
[23,24].
Natural and restored teeth are subjected to cyclic load-
ing during normal masticatory function. Therefore, the wear
process and failure due to fatigue stress are phenomena of
relevance from the clinical standpoint and should instigate
future work [25].
5. Conclusion
Higher flexural strength was produced by the 3-point bend-
ing test than by the 4-point bending test, independent of the
composite evaluated. The flexural strength and the fracture
behavior of both composites were similar, despite the dif-
ference of the average filler size of the composites tested,
probably due to the microstructural arrangement of the
nanofillers in clusters that approximate the average size of
the filler of the microhybrid composite and due to the similar
filler volume in both composites.
Acknowledgements
The authors specially thank Dr. Flávio Fernando Demarco for
his review and suggestions in the project.
This project was funded by CAPES (Coordenação de
Aperfeiçoamento de Pessoal de Nı́vel Superior), Grant no.
3640/05-1.
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