Dental Materials Journal 2008; 27(4): 541548 Original Paper

Effect of Diameter of Glass Fibers on Flexural Properties of Fiber-reinforced Composites

Motofumi OBUKURO, Yutaka TAKAHASHI and Hiroshi SHIMIZU
Division of Removable Prosthodontics, Fukuoka Dental College, 2-15-1 Tamura, Sawara-ku, Fukuoka 814-0193, Japan Corresponding author, Yutaka TAKAHASHI; E-mail: ytakaha@college.fdcnet.ac.jp

This study investigated the effect of the diameter of glass fibers on the exural properties of fiber-reinforced composites. Bar-shaped test specimens of highly filled fiber-reinforced composites (FRCs) and FRC of 30 vol% fiber content were made from a light-cured dimethacrylate monomer liquid (mixture of urethane dimethacrylate and triethylene glycol dimethacrylate) with silanized E-glass fibers (7, 10, 13, 16, 20, 25, 30, and 45 m in diameter). Flexural strength and elastic modulus were measured. The exural strength of the highly filled FRCs increased with increasing fiber diameter. In particular, the strengths of highly filled FRCs with 20-, 25-, 30-, and 45-m-diameter fibers was significantly higher than the others (p<0.05). The exural strength of FRC of 30 vol% fiber content increased with increasing fiber diameter, except for the FRC with 45-m-diameter fibers; FRCs with 20-, 25-, and 30-m-diameter fibers were significantly stronger than the others (p<0.05). Therefore, it was revealed that the diameter of glass fibers significantly affected the exural properties of fiber-reinforced composites. Key words: Fiber-reinforced composites, Flexural properties, Glass fiber diameter Received Jun 22, 2007: Accepted Jan 28, 2008

INTRODUCTION Continuous glass fibers have been investigated with a view to applying them to the reinforcement of denture base resins1-12) and repair of resin dentures13-16). Recently, fiber-reinforced composite (FRC) materials consisting of glass fibers embedded in a methacrylate resin have been used in dentistry for the frameworks of fixed partial dentures17-23) and implant-supported overdentures24), and as post materials25,26). Their clinical success depends on the strength of the FRCs, which in turn is affected by a combination of factors. The rigidity and strength of such appliances are contingent upon the polymer matrix of the FRCs and the type of fiber reinforcement27). The reinforcing capacity of the fibers, on the other hand, relies on the orientation of the fibers, the adhesion of fibers to the resin, and the impregnation of the fibers in the resin28). Furthermore, FRCs derive their strength from the inherent superior mechanical properties of the glass fibers29). In the fiber glass industry, glass fiber rovings are made by gathering a number of continuous-filament strands and winding them to form cylindrical packages30). The glass fiber strands are bundled parallel without being twisted31). Unidirectional glass fibers are fiber rovings or yarns consisting of 1,000 to 200,000 single glass fibers32). E-glass (electrical glass) fiber rovings are used in most general-purpose fiber-reinforced plastic (FRP) materials33). Filaments of continuous glass fibers range from 3 to 25 m in diameter31), and E-glass

fibers range from 5 to 15 m in diameter30). A roving consists of strands made of 10-17 m-diameter filaments31). Rovings for chopping are made from 10 m filaments, and all other rovings are made from filaments that are 13 m or coarser31). In the dental field, E-glass fibers, S-glass (high strength glass) fibers and R-glass fibers are used for commercially available FRCs29,34,35). Glass fibers in commercial FRCs are available in diameters of 11 m36), 12 m9), 15 m37), or 15-17 m38) the range of diameters similar to those of the glass fibers in industrial FRPs. It is possible that glass fibers of a certain diameter will render FRPs with optimal exural properties for dental use. The mechanical properties of commercially available FRCs have been studied9,29,35,36,39,40), but little is known about the relationship between the diameter of glass fibers and the exural properties of FRCs. As the exural properties of FRCs increase with an increase in their fiber content percentage27), it is believed that the strength of FRCs with higher fiber content will be higher. At this juncture, two related considerations must be taken into account for a holistic investigation: (1) the fiber content of FRCs may be inuenced by the diameter of glass fibers; and (2) the fiber diameter may also inuence the strength of FRCs with identical fiber content. It was hypothesized in this study that the diameter of glass fibers affects the exural properties and fiber content of the FRCs, but does not affect the exural properties of FRCs with identical fiber content. The purpose of this study was to investigate

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Table 1 Group A-7 A-10 A-13 A-16 A-20 A-25 A-30 A-45 B-7 B-10 B-13 B-16 B-20 B-25 B-30 B-45 Classification groups of the specimens Diameter of glass fiber (m) 7 10 13 16 20 25 30 45 7 10 13 16 20 25 30 45 Glass fiber content of FRC hightly filled hightly filled hightly filled hightly filled hightly filled hightly filled hightly filled hightly filled 30 vol 30 vol 30 vol 30 vol 30 vol 30 vol 30 vol 30 vol

the effect of the diameter of glass fibers on the exural properties of FRCs. MATERIALS AND METHODS Materials used Silanized E-glass fibers (7, 10, 13, 16, 20, 25, 30, and 45 m in diameter; Asahi Fiber Glass Co. Ltd., Tokyo, Japan) and a dimethacrylate monomer liquid (mixture of urethane dimethacrylate and triethylene glycol dimethacrylate) were selected as materials to be used in this study. Urethane dimethacrylate (Lot No. SH-500B, Negami Chemical Industrial Co. Ltd., Ishikawa, Japan) and triethylene glycol dimethacrylate (NK-Ester, Lot No. 0604R, Shin-Nakamura Chemical Co. Ltd., Wakayama, Japan) were mixed at a ratio of 1:1 by weight. As a light initiator, camphorquinone (Lot No. C0014, Tokyo Kasei Co. Ltd., Tokyo, Japan) and 2-dimethylaminoethyl methacrylate (Lot No. M0082, Tokyo Kasei Co. Ltd., Tokyo, Japan) were mixed at a ratio of 1:2 by weight and added to the monomer liquid at 0.7 wt. FRC specimen preparation The experimental protocol was adapted from ISO 10477:1992(E)41) for polymer-based crown and bridge materials. Each glass fiber in the bundle was impregnated with the dimethacrylate monomer liquid, and then the impregnated glass fibers were packed in a stainless steel mold (2.0 mm 2.0 mm 25.0 mm) at as high density as possible by hand. Bar-shaped specimens of each glass fiber diameter were initially polymerized in the mold under a glass cover for one minute with a light curing unit (Visio Alfa, 3M ESPE, Seefeld, Germany). After removal from the mold, the specimens were finally polymerized with a light curing unit (UniXS II, Heraeus Kulzer, Wehrheim, Germany) for three minutes. Dimensional accuracy of the specimens was verified with a micrometer at three locations within a 0.05 mm tolerance for each dimension. Ten specimens of each group (Table 1, A groups) were fabricated for the three-point exural testing and stored in air for 24 hours. Three-point bending exural test The ultimate exural strength (MPa) and elastic modulus (GPa) of the specimens were measured. Each specimen was placed on a 20-mm-long support for three-point exural testing. A vertical load was applied at the mid-point of the specimen at a crosshead speed of 1 mm/min on a load testing machine (AGS-J, Shimadzu Co., Kyoto, Japan). The exural strength (FS) (MPa) of the specimens was calculated using the following formula: FS = 3PL/2bd2

where P = maximum load, L = span distance (20 mm), b = width of the specimen, and d = thickness of the specimen. The load P was determined from each load-deection graph. Elastic modulus (E) in GPa was calculated according to the following formula: E = FL3/4bd3D where F is the load (N) at a convenient point in the straight line portion of the load-deection graph, and D is the deection (mm) at load F. All tests were performed under uniform atmospheric conditions of 23.01C and 501 relative humidity. Fiber content determination The fiber content (vol) of each glass fiber diameter of the FRCs was determined with an ashing method9,27,29,34,39). Five specimens of each FRC were desiccated for 36 hours at 37C and weighed to an accuracy of 1 mg. The specimens were then ashed for 45 minutes at 700C. Each specimen was weighed before and after ashing on an electronic scale (A 120 S, Sartorius GmbH, Goettingen, Germany). Fiber content was calculated according to the following formula: Vg = Wg/g (Wg/g + Wr/r) 100

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where Vg = volume percentage (vol) of fiber, Wg = weight percentage of fiber, g = density of fiber ( 2.55 g/cm3), Wr = weight percentage of matrix resin, and r = density of matrix resin (1.227 g/cm3). For comparison, FRCs with 30 vol fiber content of each glass fiber diameter were investigated. The weight percentages of the fibers and matrix resins were calculated. Bar-shaped specimens of 30 vol fiber content were fabricated in the same way as the bar-shaped FRC specimens, and their exural strength and elastic modulus were measured (Table 1, B groups). SEM analysis Representative specimens of the highly filled FRCs and the FRCs of 30 vol fiber content were embedded in resin and prepared for scanning electron microscopy analysis (SEM; JSM-6330F, JEOL, Tokyo, Japan). Micrographs of the cross-sections of the highly filled FRC specimens were taken at 40 and 500 magnification to study the interfacial quality between the fibers and their matrix resins. Micrographs of the cross-sections of FRC specimens with 30 vol fiber content were also taken at 40
Table 2

magnification. Fractured, highly filled FRC specimens were viewed visually. SEM micrographs of the lateral view of representative fractured specimens were taken at 200 magnification and examined for mode of fracture. Statistical analysis Data were analyzed statistically using one-way analysis of variance (ANOVA) (STATISTICA, StatSoft Inc., Tulsa, OK, USA) to examine the effects due to glass fiber diameter. Newman-Keuls post hoc comparison (STATISTICA, StatSoft Inc., Tulsa, OK, USA) was applied when appropriate at 95 confidence level. RESULTS One-way ANOVA revealed significant differences (p<0.05) in exural strength attributed to the diameter of glass fibers in the highly filled FRCs (Table 2). The exural strengths of A-20, A-25, A-30, and A-45 were significantly higher than the others (p<0.05). Post hoc analysis showed that exural strength increased with the increasing fiber diameter

Flexural strength, elastic modulus and fiber content values of the highly filled FRCs (A groups) Group A-7 A-10 A-13 A-16 A-20 A-25 A-30 A-45 Flexural strength (MPa) mean (SD) 448 (52) a 486 (40) a, b 524 (33) b 585 (54) 664 (63) c 697 (40) c 672 (33) c 700 (70) c Elastic modulus (GPa) mean (SD) 16.0 (2.4) 20.0 (3.0) a 21.9 (1.5) a, b 25.0 (1.9) c, d 23.6 (2.9) b, c 28.7 (2.0) e 26.9 (2.5) d, e 29.1 (5.1) e Fiber content (vol) mean (SD) 34.2 ( 4.9) a 41.9 ( 1.8) a, b 43.8 ( 2.8) b 53.9 ( 6.4) c 54.6 ( 8.8) c 59.0 ( 2.1) c 59.2 ( 5.5) c 63.2 (10.9) c

The same alphabet denotes no significant differences (p>0.05) Flexural strength and elastic modulus values of FRCs with 30 vol% fiber content (B groups) Group B-7 B-10 B-13 B-16 B-20 B-25 B-30 B-45 Flexural strength (MPa) mean (SD) 434 (42) a 488 (70) b 496 (53) b 511 (61) b 559 (30) c 566 (37) c 566 (45) c 415 (29) a Elastic modulus (GPa) mean (SD) 14.8 (1.4) a 13.5 (2.1) a 13.0 (2.5) a 13.1 (2.1) a 14.2 (2.1) a 15.0 (2.5) a 14.4 (1.2) a 14.8 (1.3) a

Table 3

The same alphabet denotes no significant differences (p>0.05)

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Fig. 1

Scanning electron micrographs (ah: 40 magnification; ip: 500 magnification) of the cross-sections of highly filled FRCs: (a) A-7; (b) A-10; (c) A-13; (d) A-16; (e) A-20; (f) A-25; (g) A-30; (h) A-45; (i) A-7; (j) A-10; (k) A-13; (l) A-16; (m) A-20; (n) A-25; (o) A-30; (p) A-45.

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Fig. 2

Scanning electron micrographs (40 magnification) of the cross-sections of FRCs with 30 vol% fiber content: (a) B-7; (b) B-10; (c) B-13; (d) B-16; (e) B-20; (f) B-25; (g) B-30; (h) B-45.

Fig. 3

Scanning electron micrographs (200 magnification) of the lateral view of fractured, highly filled FRC specimens: (a) A-7; (b) A-10; (c) A-13; (d) A-16; (e) A-20; (f) A-25; (g) A-30; (h) A-45. The bottom part of each specimen shows the tensile side of three-point exural testing.

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Dent Mater J 2008; 27(4): 541548 USA) and Stick (Impregnated E-glass FRC, Stick Tech, Turku, Finland) ranged from 367 to 405 MPa and from 430 to 460 MPa respectively; the elastic moduli of FibreKor and Stick were 23.8 GPa and 28.0 GPa respectively. Another study36) showed that the exural strength and elastic modulus of FibreKor were 567 MPa and 26.5 GPa respectively. In a study that examined the exural strengths of six commercially available FRCs, the values ranged from 132 MPa to 764 MPa whereby the highest was that of everStick (Preimpregnated E-glass FRC, Stick-Tech, Turku, Finland)35). The exural strength values varied among different studies because the fabrication methods were different namely the polymerization and storage conditions. On this ground, we could not compare our results with those found in published literature. Nonetheless, the exural strengths of the FRCs in the present study were on par with the highest values found for the commercially available FRCs, and the elastic modulus values were at an identical level too. The fiber content of the FRCs in this study increased with increasing fiber diameter. Scanning electron microscopic views of specimens crosssections with different fiber diameters showed good impregnation of the fibers within the resin matrix, and high filling of fiber in FRC. Fiber contents of FRCs with glass fiber diameter greater than 16 m were significantly higher than the others (p<0.05), ranging from 53.9 to 63.2 vol. On comparison with commercially available FRCs, two recent studies showed that the fiber contents of Vectris (Preimpregnated E-glass FRC, Ivoclar Vivadent, Schaan, Liechtenstein), FibreKor, and Stick were 46.5 vol, 45.2 vol, and 51.8 vol respectively29,34). In another study35), the fiber contents of Stick, everStick, Vectris, and FibreKor were 48 vol, 48 vol, 53 vol, and 38 vol respectively. Evidently, there were differences in fiber content value between these studies. In the present study, FRCs with fibers larger than 16 m in diameter yielded higher fiber content values than the commercially available FRCs. At this juncture, it behoves to put into perspective that with barshaped specimens, the number of glass fiber filaments in the FRCs gradually decreased with an increase in fiber diameter. Consequently, thicker fibers were more easily packed into a mold. Furthermore, it was thought that the impregnation of fibers with matrix resin became increasingly difficult with fibers of smaller diameters. This was because the total surface area of the fibers increased with an increase in the number of fibers. Based on the results obtained in this study, it was clearly revealed that FRCs with significantly higher fiber contents also exhibited higher exural

of the FRCs. Significant differences (p<0.05) in elastic modulus attributed to the diameter of glass fibers were also found for the FRCs. Post hoc analysis showed that the elastic modulus generally increased with increasing fiber diameter. There were significant differences (p<0.05) in the fiber content attributed to the diameter of some of the glass fibers. The fiber contents of A-16, A-20, A-25, A-30, and A45 were significantly higher than the others (p<0.05). Post hoc analysis showed that the fiber content of the FRCs increased with increasing fiber diameter. Significant differences (p<0.05) in exural strength attributed to the diameter of glass fibers were found for the FRCs with 30 vol fiber content (Table 3). The exural strengths of FRCs with 20-, 25-, and 30-m-diameter fibers were significantly higher than the others (p<0.05). Post hoc analysis showed that exural strength increased with increasing fiber diameter of the FRCs with 30 vol fiber content, except for the one with 45-m-diameter fibers. There were no significant differences (p>0.05) in elastic modulus attributed to the glass fiber diameter of FRCs with 30 vol fiber content. SEM micrographs of representative highly filled FRC specimens at 40 and 500 magnification showed the distribution of the glass fibers in the resin matrix. Impregnation of glass fibers within the resin matrix was generally good, and that the presence of voids was not observed (Fig. 1). SEM micrographs of representative FRC specimens with 30 vol fiber content showed that the fibers were not evenly distributed in the resin matrix (Fig. 2). On failure mode analysis, SEM micrographs of the fractured, highly filled FRC specimens revealed similar modes of failure (Fig. 3). Fiber fracture was the predominant mode of failure in all the specimens. Fibers remained adhered to the matrix resin after fracture, indicating good fiber-matrix bonding. Matrix resin fracture appeared to be localized where the fibers fractured. DISCUSSION The exural strength of FRCs increased with increasing fiber diameter. Flexural strength values of 20-, 25-, 30-, and 45-m-diameter fibers (ranging from 664 MPa to 700 MPa) were significantly higher than the others (p<0.05). Similarly, the elastic modulus increased with increasing fiber diameter, ranging from 23.6 GPa to 29.1 GPa for the FRCs containing fibers larger than 20 m in diameter. To date, numerous studies have been undertaken to examine the exural properties of commercially available FRCs. In a study on the exural properties of commercially available light-cured FRCs29), the exural strengths of FibreKor (Preimpregnated Sglass FRC, Pentron Corporation, Wallingford, CT,

Dent Mater J 2008; 27(4): 541548 strength. The fiber content of each FRC group with different diameters was determined by ashing, and that the content values were significantly different. Therefore, it was suggested that the exural strength of FRCs depended on both the fiber diameter and content. In a previous study, it was found that the exural properties of FRCs increased with an increase in fiber content percentage27). Likewise in this study, the fiber content significantly affected the exural strength of the FRCs. However, it remained to be confirmed if fiber diameter also made a difference in exural strength among the groups. It was thus proposed that as the fiber content of FRCs increased with increasing fiber diameter, the exural strength correspondingly increased with an increase in fiber diameter. To investigate this proposal, identical-fiber-content FRCs with different diameters were used as controls. It was reported that the mechanical properties of fiber composites depended on the direction of fibers in the polymer matrix9). In the present study, the fiber-matrix ratio of cross-sections of identical-fibercontent specimens fabricated with unidirectional glass fibers of various diameters was considered to be uniform among the specimens. During the threepoint bending test, stress was exerted perpendicular to the direction of the fibers. Hence, it was hypothesized that there would be no significant differences in the exural strength of FRCs with 30 vol glass fiber content though fabricated with various fiber diameters. However, the exural strengths of FRCs of 20, 25, and 30 m diameter were significantly higher than the others. In other words, the fiber diameter significantly affected the exural strength of FRCs of 30 vol glass fiber content. Moreover, amongst the FRCs of 30 vol glass fiber content, FRCs with significantly higher exural strength were almost identical to those of the highly filled FRCs, except for 45 m. Therefore, under the conditions of the present experiment, it was concluded that the diameter of glass fibers significantly affected the exural strength and elastic modulus of FRCs. Apart from fiber content and diameter, the inherent mechanical properties of glass fibers at each diameter also seemed to inuence exural strength. As mentioned earlier, glass fibers with diameters ranging from 10 to 17 m are generally used for FRP materials. With commercially available FRCs, glass fiber diameters generally range from 11 to 17 m. Thus, it seems reasonable that commercially available FRCs could be used as FRP materials. However, FRCs for dental use are different from industrial FRPs, which are employed for purposes such as bathtubs and train upholstery. Conversely, prostheses fabricated with FRCs are smaller and

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finer. Hence, there should be a certain diameter range of glass fibers that is appropriate for FRCs. This study indicated that better exural properties were found for the 20-30 m diameter glass fibers in the unidirectional glass fiber-reinforced composite (FRC) materials. REFERENCES
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