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Objective. To evaluate the efcacy on exural properties of owable dental resin composite
reinforced with short glass ber of different aspect ratios (ARs) and volume percent load-
ings. It is hypothesized that with the addition of randomly oriented bers it is possible to
2 April 2014
Methods. Ten groups of samples with varying glass ber volume loads (0, 5%, 10%, 20%, 40%
and 60%) and three different ARs (5.2, 68 and 640) were tested in three point bending to
fracture according to ISO 4049. A owable resin composite was used as the control and also
Keywords:
as the lled resin composite that was subsequently reinforced with bers. Load deection
Flexural
results were used to calculate exural strength and exural modulus. SEM images were
Fracture
used to determine the mode(s) of failure, to describe surface features of reinforcement and
Strength
were correlated with force displacement graphs. All results were statistically analysed using
Modulus
ANOVA followed by post hoc Tukeys test. Level of signicance was set at 0.05.
Dental composite
Results. When compared to the sculptable control (68.6 vol% ller loaded) results for ex-
Flowable
ural strength varied from a mean reduction of 42% (p > 0.05) for the low AR group to an
Glass ber
increase of 77% (p < 0.001) for the high AR samples. Flexural modulus results varied from a
Aspect ratio
low of 6.6 [0.67] GPa for the non reinforced spatulated control to 20.3 [1.31] GPa (p < 0.001) for
the 60% loaded low AR group. The low ber loaded mid AR group was still owable with 49%
total loading (5% ber/44% ller) but gave strength values (181.2 [33.5] MPa) 30% higher than
the sculptable control (p > 0.05) and comparable modulus.
Signicance. This study shows that short and very short glass bers can signicantly reinforce
owable dental composite. The bers aspect ratio was shown to be more important than volume loading for exural strength. It appears possible to produce a light cured short glass ber
reinforced owable material with superior exural properties compared to conventional
universal composites.
2014 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.
Corresponding author: Associate professor, Faculty of Dentistry, The University of Sydney, Westmead Oral Health Centre, Level 1,
Westmead Hospital, Darcy Road, Sydney, NSW 2145 Australia. Tel.: +61 298457161; fax: +61 296334759.
E-mail address: ayman.ellakwa@sydney.edu.au (A. Ellakwa) .
http://dx.doi.org/10.1016/j.dental.2014.08.363
0109-5641/ 2014 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.
d e n t a l m a t e r i a l s 3 0 ( 2 0 1 4 ) 12341244
1.
Introduction
1235
evaluated was that a owable dental composite may be signicantly reinforced by incorporating randomly distributed
short and very short glass bers. Further it was hypothesized
that, the amount of ber required to increase the exural
behavior is small thereby retaining low viscosity and owability.
2.
Ten groups (AJ) with ten samples per group were formed.
Three control groups A, B and C were not reinforced while
groups DJ formed the ber reinforced samples (Table 1). Group
A consisted of a universal high viscosity or sculptable dental composite (Beautil II, Shofu, Kyoto, Japan) while groups B
and C consisted of a low viscosity owable composite (Beautil F03 Flow Plus). Groups DF were formed by combining
this owable material (F03 Flow Plus) with low (5.2) aspect
ratio bers of different volume load fractions (20, 40 and 60%).
Groups G, H and I combined F03 Flow Plus with mid (68)
aspect ratio bers of three different loads (5, 10 and 20%)
while group J utilized high aspect ratio (640) bers with 10%
loading.
2.1.
Fibers
Glass bers with three different aspect ratios (ARs) were used
(Fig. 1). Low AR bers presented as unsized milled E glass powder from Owens Corning, Ohio, USA. SEM analysis revealed an
average length of 89 62 m (range 14300, n = 400), an average
diameter of 17 m and an AR of 5.2 3.65. They were used for
three groups (DF). High AR glass bers presented as S glass (S2 Glass) chopped strands from AGY, South Carolina, USA and
consisted of numerous 10 m diameter parallel laments cut
into short 6.4 mm lengths. These bers have an AR of 640 without deviation and were used for group J. These S glass strands
were also cut (average length 679, range 602400, n = 400) to
create the third AR of 68 43.5 used in 3 groups (GI).
Both E glass and S glass bers were used as the availability of very short cut or milled glass bers is very limited.
The prex E and S stands for electrical grade and structural grade. Their physical properties are as follows: tensile
strengths 3.4 GPa vs. 4.9 GPa, moduli 72 GPa vs. 87 GPa and
densities of 2.58 g/cc vs. 2.46 g/cc respectively. Both bers are
predominantly aluminosilicate glasses. E glass is high in calcium while S glass is high in magnesium with no boron
[19]. Given the similarity in composition, physical properties
and surface chemistry it was decided to use milled E glass
as a low AR baseline. This material is readily available and
is used by manufacturers of packable DRCs. The S glass
bers were used uncut in the higher AR sample group. The
major difference between the two glasses was thus considered to be diameter and a sufcient spread of aspect ratios was
achieved.
All bers were rst etched in a 4% potassium
dichromate(IV)(K2 Cr2 O7 )/89% sulphuric acid (H2 SO4 ) aqueous
solution (Australian Scientic, NSW, Australia) for 4 h then
thoroughly washed (until pH returned to 7) in deionized
water followed by rinsing in ethanol and drying in an oven
at 50 C for 8 h. Fibers were then immersed in a hydrolyzed
1236
d e n t a l m a t e r i a l s 3 0 ( 2 0 1 4 ) 12341244
Table 1 Ten groups (n = 10): three controls (AC); three low aspect ratio (DF); three mid AR (GI) and one high AR (J)
groups. Mean values and one standard deviation (brackets) are given. Note that only group G remained owable after
ber incorporation. ef , effective stress yielding; Eef , effective modulus.
Group
Composion
Resin
Flowability
Flexural Strength
mean
(SD)
MPa
ef
Flexural Modulus
mean (SD)
GPa
Eef
31.4
Sculptable
139.8
(10.6)
12.2
(0.74)
53.7
Low ow
126.3
(11.8)
7.6
(1.0)
53.7
Low ow
103.5
(18.3)
6.6
(0.67)
43
Paste
95.2
(15.9)
62
11
(1.11)
28.6
32.2
Paste
94.1
(11.5)
80
17
(2.02)
32.6
21.5
Packable
81.2
(19.2)
66
20.3
(1.31)
29.4
51
Flowable
181.2
(33.5)
1658
12.1
(0.94)
116.6
48.3
Paste
170.4
(28.2)
772
13.8
(2.39)
78.6
43
Paste
210.7
(48.7)
639.5
13.2
(2.85)
39.6
48.3
Paste
247.7
(75.2)
1545
13.3
(1.34)
73.6
Flowable composites are indicated in red in Flowability column. Blue and brown values relate to effective stress yielding and modulus described
on lines 364402.
2.2.
The dental composite used in this study Beautil is classied as a giomer and is composed of BisGMA/TEGDMA
resin and pre-reacted glass-ionomer (S-PRG) uoroaluminosilicate glass ller particles ranging in size from 0.01 to 4.0
(ave. 0.8) m. Manufacturers of these materials claim uoride
release and recharge capabilities while maintaining superior
physical properties to poly acid modied resin composites
(compomers) [22].
d e n t a l m a t e r i a l s 3 0 ( 2 0 1 4 ) 12341244
1237
Fig. 1 E glass (a) and S glass (b) as received from manufacturer. Cut S glass bers (c and d) showing random inter
penetrating networks.
This material is manufactured with ve viscosities depending on ller ratio ranging from 68.6% volume (83.3% by weight)
loaded sculptable Beautil II (group A) to the very low viscosity Beautil Flowable F10 (<47% by volume). Beautil Flow
Plus F03 (shade A2 lot number 111004) with 46.3% by volume
(67.3% weight) ller loading and mid viscosity was chosen as
the main control (group B) and also as the resin composite to
be reinforced with glass ber as it exhibited good strength at
low viscosity.
2.3.
Sample preparation
Weight
Density
and since,
%Vf =
Vf
Vf + Vr
Wf /f
Total Sample Volume
1238
d e n t a l m a t e r i a l s 3 0 ( 2 0 1 4 ) 12341244
3.
Testing
3PL
2wt2
4.
Results
4.1.
Flexural strength
4.2.
Flexural modulus
4.3.
Scanning electron microscopy and force
displacement graphs
Scanning electron microscopy analysis (Fig. 3) showed surface
and subsurface voids and preparation aws in all samples. The
large 400 m void in Fig. 3a resulted in a very low performance
for this sample. As expected, the spatulated control showed
much greater incidence of small and large air voids (see Figs. 3a
and b white arrows).
Scanning electron microscopy of all the controls and low
aspect ratio samples showed relatively at fracture surface
topography (see Fig. 3a and b) and correlated with brittle force
displacement graphs (Fig. 5 blue line). Photo micrographs of
10% and 20% mid aspect and all high aspect samples showed
very rough proles (Fig. 3d) and correlated with tougher force
displacement graphs (Fig. 5 green line). These samples demonstrated the presence of a deection hardening stage II which
corresponds to the onset and then saturation of ber engagement and matrix micro cracking. This stage does not exist
when ber volume is less than the critical-bending volume
and this was seen with all of the 5% mid aspect ratio samples which showed rough photo micrograph proles (Fig. 3c)
but still exhibited brittle performance in force displacement
proles.
The presence of a stage III tail is typical of further ber
debonding and pullout with associated energy expenditure.
All of the reinforced samples showed steeper inclines indicating higher modulus. Also, the end of the elastic phases
d e n t a l m a t e r i a l s 3 0 ( 2 0 1 4 ) 12341244
1239
Fig. 3 (a) Fractured surface of syringed owable control sample showing very large (400 m) surface aw (black arrow); (b)
sample from spatulated owable control group showing greater number of small (<40 m) and large (200 m) internal voids
(white arrows). Note the relatively at fracture surface topography. (c) Sample from 5% volume loaded mid AR group
showing very rough fracture surface and ber bridging (red arrows). (d) 10% volume loaded high AR overall best performing
sample. Even though this sample performed very well there was still the presence of voids and smooth ber surfaces. Note
long ber perpendicular to the long axis and near the surface acting as a stress concentrator (arrow). Also note the non
random distribution of bers. (For interpretation of the references to color in this gure legend, the reader is referred to the
web version of the article.)
aramid bers are yellow and carbon bers and nano tubes are
black.
5.2.
5.
Discussion
5.1.
Glass bers were used in this study because they are very conducive to silane bonding without the need for extra treatment.
Crystalline ceramic whiskers utilized by Xu et al. [6] required
surface fusion with nano silica particles at 800 C to achieve
effective stress transfer. Organic polyethylene bers require
plasma etching prior to silanization and still exhibit relatively
low bond strengths. The bers used in this study are also safe
to handle as they are signicantly greater than the 3 m ber
diameter considered dangerous in lung tissue and have low
biopersistence when compared to refractory ceramic bers
[23,24]. Glass bers have a refractive index much closer to
dental resins and allow for light polymerization as opposed
to crystalline whiskers, carbon bers and carbon nano bers.
The comparable refractive index also makes glass ber composites esthetic whereas whiskers at present are very opaque,
lcrit =
f d
2
1240
d e n t a l m a t e r i a l s 3 0 ( 2 0 1 4 ) 12341244
c = f Vf + m Vm
or
Ec = Ef Vf + Em Vm
a
3
and
Ec = KEf Vf + Em Vm
1241
d e n t a l m a t e r i a l s 3 0 ( 2 0 1 4 ) 12341244
Table 2 Table showing percent differences (red, negative; black, positive) in exural strength and modulus with control
groups AC. *p < 0.05, **p < 0.001.
Group
AR
Fibre vol
%
Filler
bre
total vol
%
FS %
FS %
E%
FS %
11
** 61
35
** 85
22
15
E%
E%
68.6
46.3
13
** 38
46.3
26
** 46
18
5.2
20
57.0
32
10
25
* 45
** 67
5.2
40
67.8
33
** 40
25
** 124
** 158
5.2
60
78.5
42
** 66
36
** 167
21
** 208
68
49.0
30
43
** 59
** 75
** 83
68
10
51.7
22
13
35
** 81
* 65
** 109
68
20
57.0
** 51
** 67
** 74
** 104
** 100
640
10
51.7
** 77
** 96
** 75
** 139
** 102
c (1 Vf )m
Vf
5.3.
The effect of varying the ber loading on strength and modulus of the owable composite was investigated with the 20%,
40% and 60% low aspect ratio samples (groups DF) and 5%,
10% and 20% mid aspect samples (groups GI). Note that
although containing 22.3% less ller, the owable control B
was only 13% weaker but 38% more exible than the packable
control A.
With regards to strength ber loading was not signicant
within the parameters studied in Fig. 2a showing a weakening
effect in the low aspect ratio samples. Also the low ber loaded
13
(5%) mid aspect ratio group G with only 49% combined ller
and ber loading showed a 75% (p < 0.001); 43% (p < 0.05) and a
30% (p > 0.05) improvement over the spatulated (46.3% lled),
syringed (46.3% lled) packable (68.6% lled) control groups C,
B and A. In fact, although while not signicant at p < 0.05 the
60% low aspect ratio group F showed a 36% drop over the owable control group B and a 42% drop over the packable control
group A indicating an increase in the negative inuence of
low aspect bers, i.e. matrix discontinuity and stress concentration. This effect may also be at least partly due to a greater
potential for air entrapment.
The 20% loaded mid aspect ratio group I showed a significant 67% and 51% increase over the owable and packable
controls respectively. Groups I and D with equal volumes of
bers (20%) showed marked differences in the effect of aspect
ratio with the longer bers resulting in a material twice as
strong (121% p < 0.001). Brandt [34] found that reinforcement
is proportional to ber volume but it is important to identify
a negative reinforcing effect past a certain volume. Garoushi
et al. [27] found that random short glass bers with less than
22% volume loading had a signicant strengthening effect
on dimethacrylate-polymethylmethacrylate resin based composite.
With regard exural modulus ber volume loading was proportional to modulus in the low aspect ratio systems only
(Fig. 2b). Increasing mid aspect ratio ber loading from 5% to
20% did not improve modulus beyond the 1214 GPa range possibly indicating a modulus loading dependence somewhere
above 20%. The 20% loaded mid aspect group I was 20% stiffer
than the 20% low aspect group D indicating a mild inuence of
aspect ratio on modulus. As expected signicant increases to
exural modulus was seen with all aspect ratios even at low
volume loads compared to the owable 46.3% lled control
1242
d e n t a l m a t e r i a l s 3 0 ( 2 0 1 4 ) 12341244
Fig. 5 Force displacement/stress strain curve overlays of the best performing syringed owable control (group B) sample
(blue) and best reinforced sample (from 10% high AR group J) (green). (For interpretation of the references to color in this
gure legend, the reader is referred to the web version of the article.)
5.4.
Fracture behavior
5.5.
Mixing
6.
The mixing of the mid and high aspect ratio bers resulted
in some clumping and paralleling of bers as can be seen in
Fig. 3c and d. The dispensing of a ber reinforced resin composite through a nozzle may show a similar result. Further
work may look at the inuence of ber aspect ratio, ber volume fraction and nozzle diameter in delivering a randomly
distributed ber system. In this study, viscosity was assessed
d e n t a l m a t e r i a l s 3 0 ( 2 0 1 4 ) 12341244
7.
Clinical signicance
8.
Conclusions
Acknowledgements
Ken Tyler for his time and expertise at the Biomaterials Laboratory, Sydney Dental Hospital.
The Australian Center for Microscopy and Microanalysis
(University of Sydney), in particular, Drs Ian Kaplin and Patrick
Trimby.
Shofu (Kyoto, Japan) and Horsley Dental (Australia) for their
supply of owable composite.
AGY (South Carolina, USA) for supply of S-2 glass bers.
Owens Corning (Ohio, USA) for E glass bers.
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1243
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