Art 1, Cerasmart, 130315
Art 1, Cerasmart, 130315
Art 1, Cerasmart, 130315
1
Oral Biomaterials Engineering, Department of Oral Materials Sciences and Technology, Course for Oral Health Engineering, School of Oral Health
Care Sciences, Faculty of Dentistry, Tokyo Medical and Dental University, 1-5-45 Yushima, Bunkyo-ku, Tokyo 113-8549, Japan
2
Department of Prosthodontics, Faculty of Dentistry, Chulalongkorn University, 34 Henri-Dunant Rd., Patumwan, Bangkok 10330, Thailand
3
Removable Partial Prosthodontics, Department of Masticatory Function Rehabilitation, Division of Oral Health Sciences, Graduate School of Medical
and Dental Sciences, Tokyo Medical and Dental University, 1-5-45 Yushima, Bunkyo-ku, Tokyo 113-8549, Japan
4
Comprehensive Oral Health Engineering, Department of Fundamental Oral Health Engineering, Course for Oral Health Engineering, School of Oral
Health Care Sciences, Faculty of Dentistry, Tokyo Medical and Dental University, 1-5-45 Yushima, Bunkyo-ku, Tokyo 113-8549, Japan
5
Liaison Center for Innovative Dentistry, Tohoku University Graduate School of Dentistry, 4-1 Seiryo-machi, Aoba-ku, Sendai 980-8575, Miyagi,
Japan
Corresponding author, Hidekazu TAKAHASHI; E-mail: [email protected]
This study compared commercial composite resin blocks with one ceramic block for use in computer-aided design/computer aided
manufacturing (CAD/CAM). Four composite resins, one composite ceramic, and one feldspar-ceramic block were investigated.
Flexural strength (FS), flexural modulus (FM), and Vickers hardness (VH) were determined under three conditions: dry storage;
immersion in water at 37°C for 7 days; and immersion in water at 37°C for 7 days followed by 10,000 thermocycles. After dry storage,
FS ranged from 127 to 242 MPa, FM from 9.6 to 51.5 GPa, and VH from 64 to 455. Two-way ANOVA was performed for FS, FM and
VH followed by Tukey’s multiple comparison (α<0.05). Results demonstrated that the materials degraded after water immersion
and thermocycling, but their properties were within the acceptable range for fabrication of single restorations according to the ISO
standard for ceramics (ISO 6872:2008).
Keywords: Composite resin blocks, CAD/CAM, Flexural strength, Vickers hardness, Elemental composition
Composition
Flexural Flexural
Code Filler strength modulus
Monomer MPa GPa
Composition mass%
BLO UDMA, TEGDMA Silica powder, micro fumed silica, zirconium silicate 61 191 9.5
CER Bis-MEPP, UDMA, DMA Silica (20 nm), barium glass (300 nm) 71 231 7.5
GRA UDMA, methacrylate copolymer Silica, Al-silicate glass, prepolymerized filler 76 208 11.1
Bis-GMA, UDMA, Bis-EMA, SiO2 (20 nm), ZrO2 (4–11 nm), aggregated
ULT 80 204 12.8
TEGDMA ZrO2/SiO2 cluster (SiO2 = 20 nm, ZrO2 = 4–11 nm)
ENA UDMA, TEGDMA Feldspar ceramic enriched with aluminum oxide 86 150–160 30
during flexural testing, an edge chamfer, 0.15 mm wide, to burn out the organic matrix. After cooling to ambient
was prepared using the lapping machine with a #1000 temperature in a desiccator, the residue and crucible
diamond sheet. After polishing, all specimens were were reweighed until a constant mass was obtained
stored in a desiccator with silica gel for 7 days prior to at two subsequent measurements. The inorganic filler
flexural testing. Thirty specimens of each CAD/CAM content (mass%) was determined using the following
block brand were randomly divided into three groups equation:
of ten each. Specimens from the first group were kept Filler content=(m3−m1)/(m2−m1)×100
under dry conditions at room temperature (23±2°C). The where m1 is the initial mass of the dry crucible (g); m2
second group was stored in 37°C deionized water for 7 is the initial mass of the dry crucible plus the dried
days, while the third group was stored in 37°C deionized specimen (g); m3 is the final mass of the crucible plus the
water for 7 days followed by 10,000 thermal cycles (5°C to residue after calcination (g).
55°C, dwelling time 60 s) using a thermocycling machine
(HA-K178, Tokyo Giken Inc., Tokyo, Japan). The width Filler micro-morphology and element analysis
and thickness of each specimen were measured with a After the bending test, the broken bar-shaped specimens
digital micrometer (MDC-25M, Mitsutoyo Co., Tokyo, (4.0×7.0×1.2 mm) were observed using scanning electron
Japan; minimum reading: 0.001 mm). A three-point microscopy (SEM) to evaluate the filler morphology
bending test with a support span of 12.0 mm and a and distribution. The surfaces of the specimens were
crosshead speed of 1.0 mm/min was conducted at room wet polished using SiC paper (#600, #1500, #2000, and
temperature (23±2°C) using a universal testing machine #4000) and diamond lapping films (3.0 µm and 0.3 µm)
(AG-X, Shimadzu Corp., Kyoto, Japan). The flexural and subsequently ultrasonically cleaned with acetone
strength and modulus were calculated using software for 5 min and with isopropanol for another 5 min. The
(TRAPEZIUM X, Shimadzu Corp., Kyoto, Japan). The specimens were dried, mounted on aluminum stubs, and
flexural modulus (E) was calculated using the following sputter-coated with carbon.
formula: The surface of each specimen was examined using
E=FL3/4bh3d a scanning electron microscope (SEM; S-4500, Hitachi
where F is the load at a convenient point in the straight- High-technologies Corp., Tokyo, Japan) and an energy-
line portion of the load/deflection graph, L is the span dispersive X-ray spectroscope (EDS; EMAX-7000,
distance (12.0 mm), b is the width of the specimen, h Horiba, Kyoto, Japan). SEM and EDS analyses were
is the thickness of the specimen, and d is the deflection performed on each specimen in three randomly selected
at the load F. The flexural strength (σ) was calculated areas. EDS analysis for each selected area was carried
using the following formula: out under 15 kV acceleration voltage for 100 s.
σ=3F1L/2bh2
where F1 is the maximum load during the flexural test. Statistical analysis
The flexural strength, flexural modulus and hardness
Vickers hardness test were separately analyzed with two-way analysis of
Ten fractured specimens after the flexural test from variance (ANOVA) with type of CAD/CAM block and
each group were used for the Vickers hardness test. storage conditions as the main factors, followed by
The surface hardness of the specimens was measured Tukey’s post-hoc comparisons. The filler content was
using a micro hardness testing machine (MVK-H2, analyzed using one-way ANOVA and Tukey’s post-hoc
Akashi, Kawasaki, Japan). A Vickers indenter, with comparison. The significance level was set at α=0.05.
a load of 300 gf was applied for 15 s dwell time. Five
indentations were made on each specimen and the RESULTS
hardness values were averaged.
Results of flexural strength, flexural modulus, Vickers
Measurement of filler content (by ash method) hardness, and inorganic filler content are summarized
To measure the mass percentage of inorganic filler in Table 3.
content of the CAD/CAM blocks, the standard ash The flexural strength determined after dry storage
method was used in accordance with ISO 1172:199620). ranged from 126.6 to 242.0 MPa. Flexural strength was
An alumina crucible (PC2, Nikkato, Osaka, Japan) was lower after 7-day water storage and thermocycling. Two-
kept in an electric furnace (Auto Furnace QF1, GC Corp., way ANOVA suggested that the two main factors (type
Tokyo, Japan) set at 625°C for 30 min. After cooling of CAD/CAM block and storage conditions) and their
to ambient temperature in a desiccator, the weight of interaction were significant. The flexural strength of
the crucible was measured using a precision digital BLO, CER and ULT was significantly decreased after
balance (AUW120D, Shimadzu, Kyoto, Japan; minimum 7-day water storage when compared with dry storage,
reading: 0.01 mg) until constant mass was obtained. The but not after water storage and thermocycling. The
specimens of each CAD/CAM block (approximately 1 g, flexural strength of GRA did not change significantly
n=3) were placed in the crucible, and the weight of each after 7-day water storage but was significantly lower
specimen including the crucible was measured with the after thermocycling. ENA and VIT specimens showed no
precision digital balance. The crucible with the specimen significant change in flexural strength after each of the
was heated in the electric furnace at 625°C for 30 min storage modes tested.
708 Dent Mater J 2014; 33(5): 705–710
Water 58.9 (1.6) 59.0 (1.2) 87.5 (2.7) 86.7 (1.5) 184.0 (5.9) 453.8 (7.7) B
Vickers hardness*
Water/TC 57.4 (1.5) 58.0 (0.7) 80.3 (3.1) 83.0 (1.0) 177.1 (5.2) 448.5 (19.4) A
sig a a b b c d
Filler content 61.9 (0.1) 65.0 (0.1) 70.5 (0.1) 73.1 (0.2) 86.4 (0.0) 99.8 (0.0)
(mass%) sig a b c d e f
The flexural modulus under dry conditions ranged SEM images of the CAD/CAM blocks are shown in
from 9.6 to 51.5 GPa. These values changed slightly Fig. 1. BLO exhibited two types of spherical particles,
after 7-day water storage and thermocycling. Two-way composed of silica and zirconium silicate. CER contained
ANOVA suggested that the two main factors and their relatively small and uniformly distributed particles of
interaction were significant. The flexural modulus of alumina-barium-silicate. GRA contained two distinct
BLO and ULT did not change after 7-day water storage particle types: relatively large irregularly shaped
but significantly decreased after thermocycling, whereas particles consisting mainly of silica, and relatively
the flexural modulus of GRA, CER, and ENA did not small irregularly shaped fillers consisting of potassium-
change. The flexural modulus of VIT was significantly alumina-silicate. ULT exhibited a wide range of zirconium-
greater after thermocycling than after dry storage. silicate particle sizes. ENA was characterized by a dense
The hardness of specimens kept under dry condition network structure mainly consisting of potassium-
ranged from 64.1 to 454.8. These values decreased alumina-silicate and small particles of yttrium-
after 7-day water storage and thermocycling. Two- silicate. VIT exhibited a dense network-like structure
way ANOVA suggested that the two main factors were mainly consisting of potassium-alumina-silicate, small
significant, but not their interaction. The hardness particles of yttrium-silicate and a small component of
of VIT was significantly greater than any of the other zirconium-silicate and yttrium-silicate particles probably
materials tested. The ranking of hardness figures was representing coloring agents.
as follows: VIT>ENA>ULT≥GRA>BLO≥CER. Hardness
after the three storage conditions was significantly DISCUSSION
different as follows: dry condition>7-day water
storage>thermocycling. Four composite resin blocks and one composite ceramic
The inorganic filler content was significantly block were selected and compared with a feldspar
different among all materials tested: ceramic block.
VIT>ENA>ULT>GRA>CER>BLO. According to the SEM observations, the inorganic
Dent Mater J 2014; 33(5): 705–710 709
filler content and the EDS analysis, three types of GRA and ULT were similar to that of dentin, 17.7–
structure were observed: resin matrix structure with filler 29.8 GPa23). In contrast, VIT rated a similar flexural
(BLO, CER, GRA, and ULT), ceramic network structure modulus to enamel, 72.7–105.5 GPa24,25). Seven-day
with resin matrix (ENA), and ceramic structure (VIT). water storage and thermocycling affected the flexural
Several mechanical properties may be considered for strength and flexural modulus of CAD/CAM composite
restorative material evaluation. The flexural test used resin blocks, but not those of ENA and VIT. Immersion
in this study followed the well-established and widely in water caused water penetration into the resin matrix
accepted test method described in the ISO standard11,21). of the composite resin blocks, softening the polymer15).
Three-point bending and Vickers hardness were selected Moreover, it may be hypothesized that the absorbed
as relatively simple and reliable test procedures. water would cause hydrolysis of the interfacial silane
The geometry of the three-point bending test coupling agent, especially in case of zirconium silicate that
specimens for restorative composite resins (ISO is not effectively silanized due to the high crystalline
4049:200921)) and ceramics (ISO 6872:200811)) is not content26). Accordingly, the flexural strength and
identical. Because of the limitation of the CAD/CAM modulus of zirconia-containing composite resin blocks,
block size, the geometry for ceramics was selected in especially BLO and ULT, decreased after 7-day water
this study. The flexural properties obtained from the two storage and thermocycling. However, ENA and VIT with
standard test methods were reportedly not identical but their ceramic network structure did not absorb water.
provided similar results22). Future studies regarding cyclic loading and long-term
Statistical analysis of the examined properties storage are recommended for CAD/CAM composite resin
showed significant differences among the CAD/CAM blocks.
blocks tested. Therefore, the null hypothesis that there The surface hardness of a material is a relative
was no difference in characteristics among the CAD/ measure of resistance to an external indentation force.
CAM blocks was rejected. Indentation hardness has been considered a predictor of
The results of flexural strength and modulus after the wear resistance of a material27). In several studies
dry storage and the inorganic filler contents were investigators tried to find a relationship between the
similar to the values claimed by the manufacturers. The hardness and wear resistance of composite resins.
flexural strength of CAD/CAM composite resin blocks However, the results were ambiguous28,29). Results of the
was higher than that of recently developed nanofilled two-way ANOVA of hardness values suggested that the
composite resins13). The flexural modulus results of type of material and storage conditions were significant.
710 Dent Mater J 2014; 33(5): 705–710
The changes in composite resin blocks after 7-day MN: 3M ESPE; 2000.
water storage and thermocycling could be attributed to 13) Takahashi H, Finger WJ, Endo T, Kanehira M, Koottathape
N, Komatsu M, Balkenhol M. Comparative evaluation of
water absorption in the matrix resin causing swelling
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volume, and filler/matrix coupling. J Biomed Mater Res 1998;
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of this present study suggest that restorations fabricated Dent Mater 2012; 28: 529-534.
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18) Coldea A, Swain MV, Thiel N. Mechanical properties of
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Acknowledgments
polymer-infiltrated ceramic-network material. Dent Mater
The authors would like to thank GC Corp., Shofu Inc., 2014; 30: 564-569.
20) ISO 1172: 1996. Textile-glass-reinforced plastics. Prepregs,
and 3M ESPE for donation of their materials.
moulding compounds and laminates. Determination of the
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