Characterization of porous glass fiber-reinforced composite (FRC) implant structures: porosity and mechanical properties

The aim of this study was to characterize the microstructure and mechanical properties of porous fiber-reinforced composites (FRC). Implants made of the FRC structures are intended for cranial applications. The FRC specimens were prepared by impregnating E-glass fiber sheet with non-resorbable bifunctional bis-phenyl glycidyl dimethacrylate and triethylene glycol dimethacrylate resin matrix. Four groups of porous FRC specimens were prepared with a different amount of resin matrix. Control group contained specimens of fibers, which were bound together with sizing only. Microstructure of the specimens was analyzed using a micro computed tomography (micro-CT) based method. Mechanical properties of the specimens were measured with a tensile test. The amount of resin matrix in the specimens had an effect on the microstructure. Total porosity was 59.5 % (median) in the group with the lowest resin content and 11.2 % (median) in the group with the highest resin content. In control group, total porosity was 94.2 % (median). Correlations with resin content were obtained for all micro-CT based parameters except TbPf. The tensile strength of the composites was 21.3 MPa (median) in the group with the highest resin content and 43.4 MPa (median) in the group with the highest resin content. The tensile strength in control group was 18.9 MPa (median). There were strong correlations between the tensile strength of the specimens and most of the micro-CT based parameters. This experiment suggests that porous FRC structures may have the potential for use in implants for cranial bone reconstructions, provided further relevant in vitro and in vivo tests are performed.     

Fibre-reinforced composite implant: in vitro mechanical interlocking with bone model material and residual monomer analysis

The aim of this study was to examine in vitro the mechanical interlocking of an experimental implant made of E-glass fibre-reinforced polymethyl methacrylate (PMMA)-based composite (FRC) to dental stone. FRC implants with a porous surface were embedded into the dental stone, which was chosen to simulate bone ingrowth into the porous surface of the implant, after which push-out tests were performed. PMMA cylinders with smooth and grooved surface were used as controls. In addition, the release of residual methyl methacrylate monomer (MMA) into water from FRC and control implants with different compositions and fabrication methods was determined using high performance liquid chromatography (HPLC). The highest push-out force (2149 ± 263 N) was measured for the implants with grooved surface and the lowest value for the implants with smooth surface (194 ± 68 N). The push-out forces were over five times higher for FRC implants with a porous surface (958 ± 217 N) than for implants with smooth surface. During the first day of testing, the MMA release into water was 1.4–2.8 times higher from the FRC implants than from the control PMMA implants, depending on fabrication method. With time, the difference between the implants diminished.     

In vitro antimicrobial properties of silver–polysaccharide coatings on porous fiber-reinforced composites for bone implants

Biostable fiber-reinforced composite (FRC) implants prepared from bisphenol-A-dimethacrylate and triethyleneglycoldimethacrylate resin reinforced with E-glass fibers have been successfully used in cranial reconstructions in 15 patients. Recently, porous FRC structures were suggested as potential implant materials. Compared with smooth surface, porous surface allows implant incorporation via bone ingrowth, but is also a subject to bacterial attachment. Non-cytotoxic silver–polysaccharide nanocomposite coatings may provide a way to decrease the risk of bacterial contamination of porous FRC structures. This study is focused on the in vitro characterization of the effect porosity on the antimicrobial efficiency of the coatings against Staphylococcus aureus and Pseudomonas aeruginosa by a series of microbiological tests (initial adhesion, antimicrobial efficacy, and biofilm formation). Characterization included confocal laser scanning microscopy and scanning electron microscopy. The effect of porosity on the initial attachment of S. aureus was pronounced, but in the case of P. aeruginosa the effect was negligible. There were no significant effects of the coatings on the initial bacterial attachment. In the antimicrobial efficacy test, the coatings were potent against both strains regardless of the sample morphology. In the biofilm tests, there were no clear effects either of morphology or of the coating. Further coating development is foreseen to achieve a longer-term antimicrobial effect to inhibiting bacterial implant colonization.     

纤维类型及取向对纤维-UHPC基体拔出性能影响研究

纤维与基体之间的粘结能力和机械锚固作用是基体将荷载传递给纤维的决定因素之一,不同类型的纤维和取向在拉拔时的受力形式和破坏形式决定试件承载能力。采用单根纤维拉拔试验探究了纤维类型、取向对超高性能混凝土(UHPC)界面拉伸性能的影响。结果表明:随着纤维取向的增加拔出荷载先增大后减小,在45°时拔出荷载达到最大值;随着纤维取向增加,纤维拔出时对基体破坏面积增大,纤维拔出时对于基体的破坏能力:波纹线>端勾型>直线型。由第一峰值荷载分析,波纹型钢纤维相比于直线型和端勾型钢纤维更容易脱黏。对纤维拔出时进行力学行为分析,波纹型钢纤维和端勾型钢纤维拔出过程中首先发生纤维屈服,随着荷载持续基体产生破坏,直线型钢纤维在拔出过程中最先发生纤维与基体脱黏。     

Osteoblast response to polymethyl methacrylate bioactive glass composite

Polymethylmethacrylate (PMMA) has been used in many orthopedic and dental applications since the 1960s. Biocompatibility of newly developed surface porous fiber reinforced (SPFR) PMMA based composite has not been previously proven in cell culture environment. Analysis of rat bone marrow stromal cells grown on the different test materials showed only little difference in normalized cell activity or bone sialoprotein (BSP) production between the test materials, but the osteocalcin (OC) levels remained higher (P < 0.015–0.005) through out the test with SPFR-material when compared to tissue culture poly styrene (TCPS). The cells grown on SP-FRC material also showed highest calcium depletion from the culture medium (P < 0.026–0.001) when compared to all other test substrates. SEM images of the cultured samples confirmed that all the materials enabled cell spreading and growth on their surface, but the roughened surface remarkably enhanced this process of cell attachment, division and calcified nodule formation. This study shows that the SP-FRC composite material does not elicit harmful/toxic reactions in cell cultures more than neutral TCPS and can be considered biocompatible. The material possesses good capabilities to form new mineralized tissue onto its surface, and through that a possibility to bond directly to bone. Rough surface seems to enhance osteoblast proliferation and formation of mineralized extracellular matrix.     

Acid corrosion resistance and mechanism of E-glass fibers: boron factor

Acid corrosion and stress corrosion characteristics of E-glass fibers with and without boron (B₂O₃ or B) were carefully studied, using 1 N H₂SO₄ acid at 96 °C and room temperature, respectively. The effect of boron on glass resistance to the acid attack is elucidated in conjunction with structural roles of B, Al, and Ca in the glass. Scanning electron microscopy with energy dispersive spectrometer (SEM/EDS) characterization was performed on the selective fiber samples before and after the acid leaching. For high boron-containing fibers, the results showed the formation of alteration layer enriched in Si as a result of depletion of both Ca and Al. Chemical analysis of the high boron fibers before and after 24 h acid leaching and the solution after 24 h test further confirmed that B, Ca, and Al in the glass fibers preferentially dissolved in the acid solution. Glass fiber dissolution mechanisms were discussed with a proposal that acid corrosion attack in boron-containing E-glass is controlled by hydrolysis of aluminoborate complex species (less than 10 nm) separated from the silicate glass network, whereas the acid corrosion attack in boron-free E-glass is controlled by hydrolysis of the silicate network, where 4-coordinated aluminum in the network is locally charge compensated by Ca.     

Strength degradation of glass fibers at high temperatures

This article presents an experimental investigation into the effects of temperature and heating time on the tensile strength and failure mechanisms of glass fibers. The loss in strength of two glass fiber types (E-glass and Advantex^®, a boron-free version of E-glass) was investigated at temperatures up to 650 °C and heating times up to 2 h. The tensile properties were measured by fiber bundle testing, and the maximum strength was found to be temperature and time dependent. The higher softening point of the Advantex^® fibers is reflected in superior high-temperature performance. A phenomenological model is presented for calculating the residual strength of glass fiber bundles as functions of temperature and time. The strength reduction mechanism was determined by single-fiber testing. Fracture mirror sizes on the E-glass fibers were related to the fiber strength after high-temperature treatment. Based on fracture mirror measurements, it was established that (1) the mirror constant of the glass, which reflects the network structure, does not change during heat treatment and (2) the strength degradation is a result of larger surface flaws present after heat treatment.     

Residual monomers released from glass-fibre-reinforced composite photopolymerised in contact with bone and blood

Purpose: The aim of this study was to determine the quantity of residual monomers of glass fibre-reinforced composite released into water from the composite that had been photopolymerized in contact with bone and blood. Materials and methods: E-glass fibre reinforced composite (FRC) made of E-glass fibre veil and the bis-GMA-TEGDMA-PMMA resin system was used in the study. In the first group, pieces of non-polymerised FRC were photopolymerised (40 s) in air which influenced the oxygen inhibited resin layer (positive control). In the second group, the FRC was polymerized between two glass plates allowing both surfaces to be well polymerized (negative control). In the test groups, the FRC was polymerized in contact with bone or in contact with blood. FRC specimens from all four groups were incubated in three milliliters of deionised water at 37°C for three days. At the end of the incubation period, the residual monomers were extracted from the water with dichloromethane, and the residual monomers of TEGDMA and bis-GMA quantitatively analysed by HPLC. The degree of monomer conversion was measured by FTIR from the surface of the test specimen. Differences between the groups were analysed using one-way ANOVA (p < 0.05). Results: The total quantity of residual monomers released from FRC polymerized in contact with bone was lower (0.55 wt%) than in the positive control group (0.97 wt%) (p = 0.021), and only slightly exceeded that of the negative control group (0.42 wt%) (p = 0.717). The total quantity of monomers released from FRC polymerized in contact with blood was at the level of the negative control group. The main residual monomer released was TEGDMA. The surfaces of the positive and negative controls showed a clear difference between the degree of monomer conversion, 34.0 and 62.8%, respectively, when analysed with FTIR (p < 0.001). Conclusion: The surface of the bone or contact with blood did not significantly inhibit the photoinitiated free radical polymerisation of the dimethacrylate monomer system of the FRC.     

Bonding ability evaluation of bone cement on the cortical surface of rabbit’s tibia

A composite bone cement designated G2B1 that contains β tricalcium phosphate particles was developed as a bone substitute for percutaneous transpedicular vertebroplasty. In this study, both G2B1 and commercial PMMA bone cement (CMW1) were implanted into proximal tibiae of rabbits, and their bone-bonding strengths were evaluated at 4, 8, 12 and 16 weeks after implantation. Some of the specimens were evaluated histologically using Giemsa surface staining, contact microradiography (CMR) and scanning electron microscopy (SEM). Histological findings showed that G2B1 contacted bone directly without intervening soft tissue in the specimens at each time point, while there was always a soft tissue layer between CMW1 and bone. The bone-bonding strength of G2B1 was significantly higher than that of CMW1 at each time point, and significantly increased from 4 weeks to 8 and 12 weeks, while it decreased significantly from 12 weeks to 16 weeks. Bone remodeling of the cortex under the cement was observed especially for G2B1 and presumably influenced the bone bonding strength of the cement. The results indicate that G2B1 has bioactivity, and bone bonding strength of bioactive bone cements can be estimated fairly with this experimental model in the short term.     

Study of the distribution and orientation of fibers in SFRC specimens

In steel fiber reinforced concrete (SFRC), the fibers are generally considered to be oriented isotropically. However, it is known that the procedures used in the specimen fabrication during quality control and material characterization may influence the distribution of the fibers significantly. This has an important effect on the properties determined from the specimens, which has to be considered when the results are used to analyze the behavior of other elements. In the present work, the orientation and segregation of fibers in cylindrical specimens and prisms, which are normally used in the mechanical characterization of SFRC, are evaluated. The type of compaction (i.e., table vibration, hand tamping and internal vibration) is seen to have a considerable influence on the distribution of the fibers. In the prisms, table vibration increases the tendency for the fibers to be oriented horizontally. In the cylindrical specimens, hand tamping appears to cause the least non-uniformity of the fiber distribution. The study was conducted on conventional concretes with 40 kg/m³ of fibers.     

The semi-interpenetrating polymer network matrix of fiber-reinforced composite and its effect on the surface adhesive properties

This aim of this study was to examine the effect of further-impregnation time of polymer pre-impregnated fiber-reinforcement on polymer matrix structure of the fiber-reinforced composite (FRC) used in dental applications. In addition, shear bond strength between the FRC and veneering composite after various length of further-impregnation was studied. Polymethyl methacrylate (PMMA) pre-impregnated glass fiber-reinforcement was further-impregnated with a diacrylate monomer resin by using five lengths of further-impregnation from 10 min to 24 h. The test specimens (n=5) from each five groups were treated with the solvent tetrahydrofuran and examined with a scanning electron microscope (SEM) to determinate the existence of linear PMMA in the polymer matrix of the FRC. The same lengths of further-impregnation were used to form an adhesive substrate for veneering composite and to measure the shear bond strength (n=8). The SEM examination showed that linear PMMA-polymer and cross-linked diacrylate polymer formed two independent networks for the polymer matrix of FRC. The highest mean shear bond strength value (18.7±2.9 MPa) was achieved when the fiber reinforcement was further-impregnated for 24 h. The shortest further-impregnation, 10 min, resulted in the lowest mean shear bond strength (12.7±2.9 MPa). A correlation between increased shear bond strength and longer further-impregnation was found (0.689, p<0.001). The results revealed that linear PMMA network of the polymer matrix of the FRC remained in the structure regardless of the various lengths of the further-impregnation with diacrylate resin.     

Fatigue crack propagation in polymethylmethacrylate bone cements

The fatigue crack propagation behaviour of a conventional polymethylmethacrylate (PMMA) bone cement was examined and compared with those of a low-viscosity PMMA cement and a carbon-fibre reinforced PMMA cement. The low-viscosity PMMA cement, developed for use in cement pressurization systems, did not differ significantly from conventional PMMA cement in its crack propagation behaviour. The carbon-fibre reinforced PMMA cement exhibited crack propagation rates which were approximately an order of magnitude less than those of conventional PMMA at the same range of stress intensity factor. Fractography of the test specimens revealed separation around prepolymerized PMMA beads and void formation around barium sulphate particles. Examination of carbon reinforced PMMA specimens showed poor mechanical bonding between the carbon fibres and the PMMA with considerable fibre pull-out and evidence of fibre breakage.     

Effect of fiber orientation on the structural behavior of FRP wrapped concrete cylinders

In this study, 27 concrete cylinders with a diameter of 152.4 and a height of 304.8 mm were prepared. Among them, 18 cylinders were wrapped using two layers of fiber reinforced polymer (FRP) with six fiber orientations; six cylinders were wrapped using four layers of FRP with fibers in axial or hoop direction only; the remaining three cylinders were used as control. The FRP used was E-glass fiber reinforced ultraviolet (UV) curing vinyl ester. Fifteen coupon specimens were prepared to experimentally determine the tensile strength of the FRP with fibers oriented at 0°, 45°, and 90° from the loading direction. Co-axial compression tests were conducted on the wrapped cylinders and control cylinders. The test results were compared with existing confinement models. It is found that the strength, ductility, and failure mode of FRP wrapped concrete cylinders depend on the fiber orientation and wall thickness. Fibers oriented at a certain angle in between the hoop direction and axial direction may result in strength lower than fibers along hoop or axial direction. A larger database is desired in order to refine the existing design-oriented confinement models.     

Kinetics of dissolution of glass fibre in hot alkaline solution

Kinetics of the dissolution of E-glass fibres in alkaline solutions was investigated. To allow an accurate determination of conversion, glass fibres were immersed individually in the corrosive medium and the diameter change was measured with the use of a scanning electron microscope. Few studies have been reported in the literature on the kinetics of E-glass fibre dissolution or the dissolution of individual fibres. Our experimental results fit well in the zero-order and shrinking cylinder models, suggesting either the diffusion of hydroxide ions through the solution or the glass fibre etching itself was rate-limiting step. The rate constant for the reaction of glass fibre with alkaline solution at 95 °C was found to be between 1.3 × 10^?4 and 4.3 × 10^?4 g/(m² s). The reaction order (n) was determined as 0.31–0.49 with respect to the alkaline solution, and the activation energy was 58–79 kJ/mol.     

Toughening of denture base resin with short deformable fibers

Fracture resistance of polymer reinforced with short fibers consists of a sum of contributions from matrix and fiber fracture, fiber debonding and pull-out. The existing models for predicting dependence of fracture toughness on structural variables were derived for the commercially important fiber volume fractions, i.e., for v_f ? 0.1. In this contribution, modification of the existing model for the dependence of the critical strain energy release rate, G_IC, on the fiber type, length and aspect ratio, interfacial adhesion and volume fraction has been attempted to allow predictions at low v_f < 0.10. The predictions based on the modified model were compared with experimental data on fracture toughness of lightly x-linked PMMA used to manufacture base of removable dentures toughened with short randomly oriented deformable fibers. The composite toughness was measured under impact loading to simulate typical mode of fracture of removable dentures. The G_IC for composites containing short Kevlar 29, S2-glass and poly(vinyl alcohol) (PVOH) fibers were obtained using instrumented Charpy impact tests at room temperature and impact speed of 1.0 m/s. Theoretical prediction based on the proposed model and experimental results agreed reasonably well.     

Structural effects of FRC creep

Research studies in the last 20 years allowed to obtain reliable rules for designing structures made of fiber reinforced concrete (FRC). However, design aspects like the long-term behavior of FRC, especially when synthetic fibers are adopted, require further research. Long-term behavior includes aging and creep. Aging represent the change of fiber properties into the concrete environment, which may reduce the structural bearing capacity; when present, it is an important issue for the structural safety, especially when fibers are the only reinforcement. Aging of fibers must be proven by experimental tests. Creep is a complex phenomenon, roughly considered by building codes even for traditional reinforced concrete (RC) structures. The introduction of fibers do not change anything in concrete matrix and, before cracking, in the material concrete creep behavior is not expected any change. After cracking, the structural effect of FRC creep depends on the degree of structural redundancy and on the presence of rebars since creep produces a stress redistribution in the structure or from FRC to the rebars. When FRC post-cracking resistance is necessary for equilibrium requirements, in structures with cracked sections in service conditions the structural deferred response has to be analyzed by considering the FRC creep behavior. When FRC is used for resisting secondary actions and rebars are present for equilibrium requirements, the response of a FRC element (with rebars and fibers) will be identical to a conventional RC; FRC contributes by controlling the crack development under both short and long term loading.     

Improvement of Mechanical Properties of Oligomer-modified Acrylic Bone Cement with Glass-fibers

Some mechanical properties of oligomer-modified acrylic bone cement with glass-fibers were studied. Under wet environments, oligomer-filler forms a porous structure in the acrylic bone cement. Test specimens were manufactured using commercial bone cement (Palacos^® R) with different quantities of an experimental oligomer-filler (0–20 wt%), and included continuous unidirectional E-glass fibers (l=65 mm) or chopped E-glass fibers (l=2 mm). The specimens were either tested dry, or after being immersed under wet environments for one week. The three-point bending test was used to measure the flexural strength and modulus of the acrylic bone cement composites (analysis with ANOVA). A scanning electron microscope (SEM) was used to examine the surface structure of the acrylic bone cement composites. Using continuous glass-fiber reinforcement, the dry flexural strength was 145 MPa and modulus was 4.6 GPa for the plain bone cement. For the test specimens with 20 wt% of oligomer-filler and continuous unidirectional glass-fibers, the dry flexural strength was 118 MPa and modulus was 4.2 GPa, whereas the wet flexural strength was 66 MPa and modulus was 3.0 GPa. The results suggest that the reduced flexural properties caused by the porosity of oligomer-modified bone cement can be compensated with glass-fiber reinforcement.     

Load bearing capacity of bone anchored fiber-reinforced composite device

The purpose of this study was to evaluate the push-out load-bearing capacity of threaded fiber-reinforced composite (FRC) devices for use as bone-anchored devices. The purpose was also to evaluate the possibility to use bioactive glass (BAG) granules on the experimental FRC devices in terms the mechanical behavior. Three experimental FRC devices (n = 15) were fabricated for the study: (a) threaded device with smooth surface; (b) threaded device with BAG granules (S53P4, Vivoxid Ltd, Turku, Finland) and supplementary retention grooves, and (c) unthreaded device with BAG granules. Threaded titanium devices were used as controls. The FRC devices were prepared from a light-polymerized dimethacrylate resin reinforced with preimpregnated unidirectional and bidirectional E-glass fibers (EverStick, StickTech Ltd, Turku, Finland). Experimental and control devices were embedded into dental plaster to simulate bone before the mechanical push-out test was carried out. ANOVA and Weibull analysis were used for the statistical evaluation. Threaded FRC devices had significantly higher push-out strength than the threaded titanium device (p < .001). The push-out forces exceeding 2,500 N were measured for threaded FRC devices with supplementary grooves and BAG coating. No thread failures were observed in any FRC devices. The unthreaded FRC devices with BAG lost 70% of glass particles during the test, while no BAG particles were lost from threaded FRC devices. It can be concluded that threaded FRC devices can withstand high push-out forces in the dental plaster without a risk of thread failure under physiological load.     

Influence of fiber chemical coating on the acoustic emission behavior of steel fiber reinforced concrete

The current study focuses on the effect of chemical coating on the acoustic emission (AE) characteristics monitored during the fracture process in steel fiber reinforced concrete (SFRC). Different shapes of chemically treated and un-treated steel fibers are used to create specimens which are subjected to four point bending up to failure. Sensitive AE indices demonstrate that the coating gives distinct characteristics to the interface bonding between the fiber and the concrete matrix, which are evident mainly during the pull-out stage, after the moment of macroscopic crack formation. Specifically, AE average frequency and RA value, which defines the rising angle of the waveforms indicate that coating results in extensive matrix cracking in addition to the friction between fiber and concrete which characterizes the uncoated fibers. AE analysis can be used for interpretation of the fracturing stage and characterization of the fracture mode. It is shown that the surface conditioning of the fibers leaves a clear fingerprint on the AE signals, shedding light into the processes that occur during failure in SFRC.     

Study of trimming damages of CFRP structures in function of the machining processes and their impact on the mechanical behavior

The main focus of this paper is to investigate the defects generated by different machining processes (namely burr tool machining, abrasive water jet machining ‘AWJM’ and abrasive diamond cutter ‘ADS’) and their impact on the mechanical behavior of CFRP in quasi-static (compression and inter-laminar shear) and tensile–tensile fatigue tests. The cutting conditions are selected so that different levels of degradation can be obtained. The machined surface is characterized using roughness measuring devices with and without contact and SEM observations. The results show that the defects generated during the trimming process with a cutting tool are fibers pull-out and resin degradation. These defects are mainly located in the layers with the fibers oriented at −45° and 90°. However, when using abrasive water jet and abrasive diamond processes, the defects generated have the form of streaks and are not dependent on the fiber orientation. Furthermore, the results of quasi-static tests performed on specimens machined by cutting tools show that AWJ specimens offer a better resistance in compression but the ADS samples offer higher inter-laminar-shear strengths. Moreover, the results of fatigue tests show that specimens machined with a burr tool offer higher endurance limit. Finally, it is concluded that the type and the mode of the mechanical loading (quasi-static fatigue) affect the mechanical response of CFRP and favor a given machining process.