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Comparison of Mechanical Properties of T PDF
Comparison of Mechanical Properties of T PDF
This work was done in partial fulfillment of the requirements of the degree of Advanced Diploma in Prosthodontics for Brian T. W. Leung at the Faculty of Dentistry,
The University of Hong Kong.
a
Postgraduate student, Oral Rehabilitation, Faculty of Dentistry, The University of Hong Kong, Hong Kong, PR China.
b
Assistant Professor, Dental Materials Science, The University of Hong Kong, Hong Kong, PR China.
c
Associate Professor, Dental Materials Science, The University of Hong Kong, Hong Kong, PR China.
d
Clinical Associate Professor, Oral Rehabilitation, The University of Hong Kong, Hong Kong, PR China.
In(In(1/(1-F)))
Experimental FGC 18.34 121.00 107.03 10
m, Weibull modulus parameter; h, 63.2% of investigated populations expected to fail; B10, 5
10% of investigated populations expected to fail; FGC, fluorophlogopite glass ceramic.
0
–5
100 –10
IPS e.max CAD
90 Vitablocs Mark II –15
Vita Enamic
Probability of Failure (%)
80 FGC –20
4.2 4.4 4.6 4.8 5 5.2 5.4 5.6 5.8 6
70
In(δδ)
60
Figure 2. Weibull plots of 4 ceramics tested.
50
40
30 reflect an early clinical failure. The aim of this study was
20 to compare the mechanical properties of 3 commercially
available ceramics with an experimental FGC.
10
0
0 50 100 150 200 250 300 350 400 450 MATERIAL AND METHODS
Flexural Strength (MPa) The ceramic specimens, batch numbers, and manufac-
Figure 1. Probability of failure versus flexural strength. turers are listed in Table 1. All the ceramic materials were
used as supplied.
A 3-point bend test was used to evaluate flexural
ceramics are being evaluated. The 3-point bending test strength. Ceramic blocks were sectioned into dimension of
has been used as a standard test for measuring flexural approximately 2×2×15 mm with a cutting machine (Micro
strength. However, the strength of ceramic is a complex Slice; Metals Research) using an alloy blade. Fifteen
parameter that cannot be fully described by a single specimens were prepared for each ceramic. Each specimen
value. The maximum flexural strength varies greatly from was further polished with 180-, 400-, 600- and 1200-grit
specimen to specimen because of the distribution of flaws SiC papers and a polishing machine (ECOMET 5; Bueh-
present in the specimen.36 When flaws are consistent ler) under running water for 10 minutes. For IPS e.max
and evenly distributed, the flexural strength of a spec- CAD, final sintering was carried out in a furnace (Pro-
imen will behave more consistently than when flaws are gramat CS; Ivoclar Vivadent AG) according to the manu-
clustered inconsistently.36 Thus, the Weibull theory could facturer’s instructions. The specimens were stored dry for 1
provide a useful description of the intrinsic statistical week until tested. The final dimensions of each specimen
variation in the fracture stress behavior of ceramic.36 were measured with a digital caliper (Digimatic Caliper;
The Weibull distribution is a generalization of the Mitutoyo). Then the specimens were mounted on a uni-
exponential distribution that describes the survival and versal loading machine (ElectroPuls E3000; Instron In-
failures times of brittle materials. Analyzing failure dustrial Products). The specimen was placed centrally on a
probability with the Weibull distribution could help to 3-point bending stand with a supporting distance of 10
understand the life time of the materials better than mm. A testing load was applied at a crosshead speed of 1
using the material strength alone.41,42 The Weibull mm/min until the specimen fracture.
modulus (m) is not a material constant but reflects the For surface hardness testing, ceramic blocks of approx-
shape of the defect population present in the material.43 imately 14×12×4 mm were sectioned, polished, and sin-
It is understood that the higher the Weibull modulus, the tered as described in the first experiment. Five Vickers
less variation. The Weibull scale parameter is known as hardness indentations were made per specimen with a
the characteristic life or characteristic strength that could hardness tester (microhardness tester; Leitz) and analyzed
estimate or reflect the failure statistically. In particular, 2 by software (Leica QGo; Leica Microsystems Imaging So-
failure percentages are usually used: h denotes the esti- lution) using a 1.96 N load and a dwell time of 15 seconds.
mated 63.2% of investigated population that would fail, The mean hardness value was calculated for each specimen.
and B10 denotes the 10% of the investigated population After the 3-point bending test, all fractured specimens
that could fail. B10 is a parameter that might be able to were examined by using scanning electron microscopy
Figure 3. Scanning electron microscope images of specimens at fractured surface after flexural strength test (×100). A, IPS e.max CAD. B, Vitablocs Mark
II. C, Vita Enamic. D, Experimental fluorophlogopite glass ceramic.
(SEM) (Hitachi S-3400N VP-SEM; Hitachi High- II group (106.67 ±18.50 MPa) and the FGC group (117.61
Technologies). Energy-dispersive x-ray analysis was ±7.62 MPa). However, no significant difference in flexural
also performed to investigate the elemental composition strength was found between the Vitablocs Mark II group
of the tested specimen. and FGC group (P=.577).
Data were analyzed by statistical software (SPSS A significant difference in Vickers hardness was found
Statistics v20 for Windows; IBM Corp). Differences in among the groups (P<.001). After adjusting for multiple
flexural strength and hardness among groups were comparisons, the Vickers hardness of the ceramics was found
analyzed by 1-way ANOVA with the Bonferroni correc- to be of the following order: IPS e.max CAD (731.63 ±30.64
tion to adjust for multiple comparisons (a=.05). The HV)>Vitablocs Mark II (594.74 ±25.22 HV)>Vita Enamic
Weibull modulus and the Weibull characteristic strength, (372.29 ±51.23 HV)>FGC (153.74 ±23.62 HV) (P<.05).
which is the strength that occurs at a probability that a The data of the Weibull parameters, including the
specimen would fail, were determined with a spread- Weibull modulus (m), the 63.2% of the specimens ex-
sheet (Excel 2010 for Windows; Microsoft Corp). pected to fail (h), and the 10.0% of the specimens ex-
pected to fail (B10), are presented in Table 3. The Weibull
plots are shown in Figures 1, 2. The Weibull plot revealed
RESULTS
that IPS e.max CAD>Vita Enamic>FGC>Vitablocs Mark
Table 2 represents the flexural strength and Vickers II for a characteristic strength at both 63.2% (h) and
hardness of each ceramic type. A significant difference in 10.0% (B10). The Weibull modulus ranged from 6.925 to
flexural strength was found among the groups (P<.001). 18.338, and the FGC showed the highest Weibull
After adjusting for multiple comparisons, the flexural modulus among the 4 studied ceramic materials.
strength of the IPS e.max CAD group (341.88 ±40.25 Figure 3 shows the SEM images of different ceramic
MPa) was found to be significantly higher (P<.001) than materials after the 3-point bend test. The fracture sur-
the Vita Enamic group (145.95 ±12.65 MPa), which was faces of Vita Enamic and experimental FGC appeared
also significantly higher (P<.001) than the Vitablocs Mark rougher compared with Vitablocs Mark II and IPS e.max
Table 4. Energy-dispersive x-ray analysis The Weibull modulus (m) of all groups was larger than 1,
App Intensity Weight% which indicates that the failure rate increases with time.
Element Conc Correlation Weight% Sigma Atomic%
Although the flexural strength of FGC is lower than that
IPS e.max CAD
CK 4.68 0.26 6.71 1.21 10.79
of Vita Enamic and IPS e.max CAD, it presented with the
OK 122.03 0.87 51.63 0.71 62.34
highest Weibull modulus among the 4 materials, sug-
Al K 8.43 1.51 2.03 0.07 1.47 gesting that the FGC material has less quality variability
Si K 81.92 0.94 32.31 0.46 22.22 than other tested ceramics. To improve the flexural
PK 4.25 0.93 1.68 0.08 1.05 strength of FGC, previous studies had shown that by
KK 10.02 0.97 3.81 0.08 1.88 varying the chemical composition, such as the fluoride
Ce L 3.8 0.78 1.80 0.14 0.25 content,38 addition of zirconia,37 heat treatment condi-
Totals 100.00 tions,37 the flexural strength can be increased up to
Vitablocs Mark II 228.11 MPa. Furthermore, Vita Enamic, a polymer-
CK 3.28 0.25 4.91 3.80 8.17 containing ceramic, also has a higher Weibull modulus
OK 99.21 0.83 44.88 1.81 56.08 than Vitablocs Mark II and IPS e.max CAD. Brittle
Na K 13.95 0.92 5.66 0.25 4.92 materials, such as the traditional dental ceramics, can
Al K 48.72 1.51 12.07 0.50 8.94
usually be described by the Griffith behavior theory.44
Si K 57.97 0.82 26.38 1.07 18.78
However, the existence of the polymer phase within
KK 14.79 0.98 5.65 0.24 2.89
the ceramic phase gives the onset of plasticity to the bulk
Ca K 1.12 0.92 0.45 0.06 0.23
Totals 100.00
material and thus can demonstrate another possible
Vita Enamic
model: the Dugdale cracking model.31 In brief, polymer
CK 46.26 0.40 35.55 2.04 47.76 chains in the polymer phase in Vita Enamic could spread
OK 67.10 0.58 35.10 1.15 35.41 the plasticity under the increase of load and hence
Na K 9.36 0.91 3.12 0.12 2.19 increase the crack resistance with the crack length. This
Al K 36.36 1.53 7.20 0.24 4.31 could give a higher observable Weibull modulus, rather
Si K 44.30 0.88 15.32 0.50 8.80 than toughening itself.32 Thus, the Vita Enamic might not
KK 11.68 1.00 3.53 0.13 1.46 have a higher toughness than others; rather the Dugdale
Ca K 0.55 0.94 0.18 0.04 0.07 behavior lowered the scattering in flexural strength
Totals 100.00 values for a given sampling population and therefore
Experimental FGC increased the Weibull modulus. Nevertheless, further
CK 12.77 0.32 13.59 1.09 20.98 clarification of the behavior and the material relationship
OK 90.99 0.75 41.48 0.61 48.10
is necessary.
FK 3.080 0.20 5.31 0.29 5.19
Hardness is defined as the resistance to a permanent
Mg K 17.21 0.79 7.44 0.14 5.68
surface indentation. In ceramics, hardness affects the
Al K 32.16 1.37 8.06 0.15 5.55
Si K 38.76 0.81 16.47 0.25 10.88
polishability, wear resistance, and ease of milling.45
KK 22.31 1.00 7.65 0.14 3.63
Because an ideal dental restorative material should not
Totals 100.00 wear the opposing dental tissues, a ceramic with a high
hardness value might not be desirable. Although the
App Conc: apparent concentration; FGC, fluorophlogopite glass ceramic.
Vickers hardness values of FGC and Vita Enamic were
low compared with other tested ceramics, their values are
comparable with enamel (611.8 Hv) and dentin (102
CAD. Energy-dispersive x-ray analysis confirmed that
Hv).46-48 Therefore, FGC and Vita Enamic might be
the chemical components were the same as those
considered as nonaggressive to opposing tooth structure,
claimed by the manufacturers, except that Ti was not
although wear is a complicated process and is not
found in Vitablocs Mark II or Vita Enamic, and Zr was
determined by material hardness only.
not detected in IPS e.max CAD (Table 4, Fig. 4).
The majority of the results in this study are compa-
Furthermore, the carbon weight percentage was higher in
rable with the data from manufacturers (Table 2) and
Vita Enamic than others, which might be explained by
other in vitro studies,27,28 except the IPS e.max CAD
the methacrylate polymer component, and fluoride was
flexural strength (137.51 MPa) in 1 study.28 The observed
present in the experimental FGC. Ce was also found in
discrepancy might be due to the differences in the
IPS e.max CAD (Table 4, Fig. 4).
preparation of the materials. For example, Charlton
et al28 tested specimens of size 4×3×18 mm with sup-
DISCUSSION
porting rollers set at 14 mm apart, which is different from
This study compared the flexural strength, Vickers the present study (specimen size of 2×2×15 mm with the
hardness, and Weibull parameters of 3 commercially supports set at 10 mm apart). Data for FGC are still
available millable ceramics against an experimental FGC. limited. Studies37,38 have shown variations in flexural
Si
Si
Al
O O
Ca
C C Na K
Al P K Ce
K Ce Ce Ce Ce K Ca
0 2 4 6 8 10 0 2 4 6 8 10
Full Scale 13903 cts Cursor: 0.000 keV' Full Scale 10106 cts Cursor: 0.000 keV'
A B
Si Si
O O Al
C Al Mg
K K
F
Ca
Na K C
Ca K
0 2 4 6 8 10 0 2 4 6 8 10
Full Scale 7572 cts Cursor: 0.000 keV' Full Scale 6684 cts Cursor: 0.000 keV'
C D
Figure 4. Energy-dispersive x-ray spectroscopic analysis of representative specimens. A, IPS e.max CAD. B, Vitablocs Mark II. C, Vita Enamic. D,
Experimental FGC.
strength from 80.6 MPa to 228.11 MPa, compared with interfaces in Vita Enamic30 or by the flake component
117.61 MPa obtained in the current study. Vickers in FGC.37 This behavior is an indication of the damage
hardness also varies among studies37,38,40 from 0.58 Hv tolerance of Vita Enamic and FGC. Clinically, local
to 836.1 Hv, compared with 153.74 Hv in the current damage deriving from milling or clinical adjustment may
study. Thus, varying the composition and conditions, be less likely to result in chipping.30
such as heat treatment, may produce different materials In summary, the experimental FGC is the least
with various properties, and therefore no direct com- abrasive ceramic with the highest Weibull modulus
parison can be made. compared with the other tested ceramics. Because it is
The SEM images of the fractured slot surfaces etchable and possesses a fluoride-releasing property,
revealed differences among the materials. Depending on FGC might be an alternative to dental ceramic. However,
the differences in the microstructure, the appearance of further development is needed to improve its flexural
the fracture pattern and fracture surfaces differ. The strength and optical properties.
fracture surfaces of Vita Enamic and experimental FGC
were rougher compared with Vitablocs Mark II and IPS
CONCLUSIONS
e.max CAD. The smooth fractured surfaces imply crack
propagation with a limited deflection. Coldea et al30 The flexural strength and Vickers hardness of IPS e.max
suggested that “propagating cracks are deflected and CAD were significantly higher than that of the 3 mate-
experience a more tortuous path . resulting in rough rials tested. FGC’s flexural strength was comparable with
surfaces.” This suggests that cracks induced by stress run Vitablocs Mark II. FGC’s Weibull modulus was the
through the ceramic parts in Vitablocs and IPS e.max highest, while its Vickers hardness was the lowest among
CAD ceramic but deflect more at the polymer-ceramic the materials tested.