Size-controlled hydroxyapatite nanoparticles as self-organized organic-inorganic composite materials

This paper presents some results concerning the size-controlled hydroxyapatite nanoparticles obtained in aqueous media in a biopolymer matrix from soluble precursors salts. Taking the inspiration from nature, where composite materials made of a polymer matrix and inorganic fillers are often found, e.g. bone, shell of crustaceans, shell of eggs, etc., the feasibility on making composite materials containing chitosan and nanosized hydroxyapatite was investigated. A stepwise co-precipitation approach was used to obtain different types of composites by means of different ratio between components. The synthesis of hydroxyapatite was carried out in the chitosan matrix from calcium chloride and sodium dihydrogenphosphate in alkaline solutions at moderate pH of 10-11 for 24 h. Our research is focused on studying and understanding the structure of this class of composites, aiming at the development of novel materials, controlled at the nanolevel scale. The X-ray diffraction technique was employed in order to study the kinetic of hydroxyapatite formation in the chitosan matrix as well as to determine the HAp crystallite sizes in the composite samples. The hydroxyapatite synthesized using this route was found to be nano-sized (15-50 nm). Moreover, applying an original approach to analyze the (002) XRD diffraction peak profile of hydroxyapatite by using a sum of two Gauss functions, the bimodal distribution of nanosized hydroxyapatite within the chitosan matrix was revealed. Two types of size distribution domains such as cluster-like (between 200 and 400 nm), which are the habitat of 'small' hydroxyapatite nanocrystallites and scattered-like, which are the habitat of 'large' hydroxyapatite nanocrystallites was probed by TEM and CSLM. The structural features of composites suggest that self-assembly processes might be involved. The composites contain nanosized hydroxyapatite with structural features close to those of biological apatites that make them attractive for bone tissue engineering applications.     

Hydroxyapatite-polyethylene composites for bone substitution: effects of ceramic particle size and morphology

Synthetic hydroxyapatite particles of two median sizes and different morphologies have been used to manufacture hydroxyapatite reinforced high density polyethylene composites (HAPEX^TM) for medical applications. The effects of hydroxyapatite particle size on properties of the resultant composites were investigated using various techniques. It was found that composites with smaller hydroxyapatite particles had higher torsional modulus, tensile modulus and tensile strength, but lower strain to failure. Examination of fracture surfaces revealed that only a mechanical bond existed between the filler and the matrix. It was shown that dynamic mechanical analysis is useful in studying the viscoelastic behaviour of the composite.     

Solvent-free polymer/bioceramic scaffolds for bone tissue engineering: fabrication,analysis, and cell growth

This study examines the potential use of porous polycaprolactone (PCL) and polycaprolocatone/hydroxyapatite (PCL/HA) scaffolds fabricated through melt molding and porogen leaching for bone tissue engineering. While eliminating organic solvents is desirable, the process steps proposed in this study for uniformly dispersing HA particles (~5?μm in size) within the scaffold can also contribute to homogeneous properties for these porous composites. Poly(ethylene oxide) (PEO) was chosen as a porogen due to its similar density and melting point as PCL. Pore size of the scaffold was controlled by limiting the size of PCL and PEO particles used in fabrication. The percent of HA in the fabricated scaffolds was quantified by thermogravimetric analysis (TGA). Mechanical testing was used to compare the modulus of the scaffolds to that of bone, and the pore size distribution was examined with microcomputed tomography (μCT). Scanning electron microscopy (SEM) was used to examine the effect on scaffold morphology caused by the addition of HA particles. Both μCT and SEM results showed that HA could be incorporated into PCL scaffolds without negatively affecting scaffold morphology or pore formation. Energy-dispersive X-ray spectroscopy (EDS) and elemental mapping demonstrated a uniform distribution of HA within PCL/HA scaffolds. Murine calvaria-derived MC3T3-E1 cells were used to determine whether cells could attach on scaffolds and grow for up to 21 days. SEM images revealed an increase in cell attachment with the incorporation of HA into the scaffolds. Similarly, DNA content analysis showed a higher cell adhesion to PCL/HA scaffolds.     

Development and in vitro characterisation of novel bioresorbable and bioactive composite materials based on polylactide foams and Bioglass for tissue engineering applications

Bioactive and bioresorbable composite materials were fabricated using macroporous poly(DL-lactide) (PDLLA) foams coated with and impregnated by bioactive glass (Bioglass) particles. Stable and homogeneous Bioglass coatings on the surface of PDLLA foams as well as infiltration of Bioglass particles throughout the porous network were achieved using a slurry-dipping technique in conjunction with pre-treatment of the foams in ethanol. The quality of the bioactive glass coatings was reproducible in terms of thickness and microstructure. Additionally, electrophoretic deposition was investigated as an alternative method for the fabrication of PDLLA foam/Bioglass composite materials. In vitro studies in simulated body fluid (SBF) were performed to study the formation of hydroxyapatite (HA) on the surface of PDLLA/Bioglass composites. SEM analysis showed that the HA layer thickness rapidly increased with increasing time in SBF. The high bioactivity of the PDLLA foam/Bioglass composites indicates the potential of the materials for use as bioactive, resorbable scaffolds in bone tissue engineering.     

Effect of Biopolymers on Structure of Hydroxyapatite and Interfacial Interactions in Biomimetically Synthesized Hydroxyapatite/Biopolymer Nanocomposites

The interfacial interaction and effect of biopolymer on crystal structure of hydroxyapatite in biomimetically synthesized nanocomposites, chitosan/hydroxyapatite (ChiHAP50), polygalacturonic acid/hydroxyapatite (PgAHAP50), and chitosan/polygalacturonic acid/hydroxyapatite (ChiPgAHAP50) have been investigated using atomic force microscopy (AFM), Fourier transform infrared (FTIR) spectroscopy, and Rietveld analysis. AFM phase images show nano-sized hydroxyapatite particles uniformly distributed in biopolymer. FTIR spectra indicate that chitosan interacts with hydroxyapatite through NH₃ ⁺ groups, whereas in polygalacturonic acid/hydroxyapatite, dissociated carboxylate groups (COO⁻) form unidentate chelate with calcium atoms. A change in lattice parameters of hydroxyapatite in all nanocomposites is observed using Rietveld analysis. The increase in lattice parameters was most prominent along c-axis in ChiHAP50 and ChiPgAHAP50 nanocomposites, which was 0.388% and 0.319%, respectively. Comparison between particle sizes of hydroxyapatite, determined from AFM and Rietveld analysis, indicates presence of amorphous phase in hydroxyapatite particles, which is believed to be present at the interface of hydroxyapatite and biopolymer.     

In vitro bioactivity of S520 glass fibers and initial assessment of osteoblast attachment

Bioactive glass fibers are attractive materials for use as tissue-engineering scaffolds and as the reinforcing phase for resorbable bioactive composites. The bioactivity of S520 glass fibers (52.0 mol % SiO(2), 20.9 Na(2)O, 7.1 K(2)O, 18.0 CaO, and 2.0 P(2)O(5)) was evaluated in two media, simulated body fluid (SBF) and Dulbecco's modified Eagle's medium (DMEM), for up to 20 days at 37 degrees C. Hydroxyapatite formation was observed on S520 fiber surfaces after 5 h in SBF. After a 20-day immersion, a continuous hydroxyapatite layer was present on the surface of samples immersed in SBF as well as on those samples immersed in DMEM [fiber surface area to solution volume ratio (SA:V) of 0.10 cm(2)/mL]. Backscattered electron imaging and EDS analysis revealed that the hydroxyapatite layer formation was more extensive for samples immersed in SBF. Decreasing the SA:V ratio to 0.05 cm(2)/mL decreased the time required to form a continuous hydroxyapatite surface layer. ICP was used to reveal Si, Ca, and P release profiles in DMEM after the 1st h (15.1, 83.8, and 29.7 ppm, respectively) were similar to those concentrations previously determined to stimulate gene expression in osteoblasts in vitro (16.5, 83.3, and 30.4 ppm, respectively). The tensile strength of the 20-microm diameter fibers was 925 +/- 424 MPa. Primary human osteoblast attachment to the fiber surface was studied by using SEM, and mineralization was studied by using alizarin red staining. Osteoblast dorsal ruffles, cell projections, and lamellipodia were observed, and by 7 days, cells had proliferated to form monolayer areas as shown by SEM. At 14 days, nodule formation was observed, and these nodules stained positive for alizarin red, demonstrating Ca deposition and, therefore mineralization.     

Poly(ethylene glycol) hydrogels cross-linked by hydrolyzable polyrotaxane containing hydroxyapatite particles as scaffolds for bone regeneration

Poly(ethylene glycol) (PEG) hydrogels cross-linked by a hydrolyzable polyrotaxane containing hydroxyapatite particles (PRX-HAp) were developed as scaffolds for bone regeneration. Five scaffolds with various composition of the polyrotaxane, PEG and HAp particles were prepared to examine cell adhesion in vitro using rat primary cultured osteoblast. Cells were observed to attach well on a PRX-HAp that have the same weight ratio of the polyrotaxane and HAp particles at 7 days after seeding. These results indicate that HAp particles are necessary for cell adhesion and survival, but a higher ratio of the particles is not suitable for cell adhesion. The composites of rat osteoblast and the PRX-HAp were implanted subcutaneously in syngeneic rats and harvested at 5 weeks after implantation. In histological analysis, osteoblast-like cells became arrayed along the surface of the PRX-HAp, and osteoid-like tissues were observed in the region between a queue of osteoblast-like cells and PRX-HAp. These images are similar to intramembranous ossification, and it is expected that bone regeneration occurs on the surface of the PRX-HAp. This study strongly suggests the great potential of the PRX-HAp as scaffolds for bone regeneration.     

Poly(ethylene glycol) hydrogels cross-linked by hydrolyzable polyrotaxane containing hydroxyapatite particles as scaffolds for bone regeneration

Poly(ethylene glycol) (PEG) hydrogels cross-linked by a hydrolyzable polyrotaxane containing hydroxyapatite particles (PRX-HAp) were developed as scaffolds for bone regeneration. Five scaffolds with various composition of the polyrotaxane, PEG and HAp particles were prepared to examine cell adhesion in vitro using rat primary cultured osteoblast. Cells were observed to attach well on a PRX-HAp that have the same weight ratio of the polyrotaxane and HAp particles at 7 days after seeding. These results indicate that HAp particles are necessary for cell adhesion and survival, but a higher ratio of the particles is not suitable for cell adhesion. The composites of rat osteoblast and the PRX-HAp were implanted subcutaneously in syngeneic rats and harvested at 5 weeks after implantation. In histological analysis, osteoblast-like cells became arrayed along the surface of the PRX-HAp, and osteoid-like tissues were observed in the region between a queue of osteoblast-like cells and PRX-HAp. These images are similar to intramembranous ossification, and it is expected that bone regeneration occurs on the surface of the PRX-HAp. This study strongly suggests the great potential of the PRX-HAp as scaffolds for bone regeneration.     

Morphological and X-ray diffraction studies of crystalline hydroxyapatite-reinforced polycaprolactone

Morphological and mechanical properties of hydroxyapatite (HAP)-reinforced polycaprolactone (PCL) were studied. The objective was to examine how morphological features alter the bulk mechanical properties in our laboratory-synthesized HAP-reinforced PCL. HAP crystals were synthesized by hydrolysis of mixtures of calcium and phosphate salts in the laboratory with wet chemical methods. The properties of the commercially available hydroxyapatite (HAP(1)) are compared with that of laboratory-synthesized hydroxyapatite (HAP(2)). The HAP crystals and composition were characterized using X-ray diffraction, scanning electron microscopy, transmission electron microscopy, and Fourier transform infrared spectrometry (FTIR). The HAP(1) and HAP(2) crystals were dispersed into polymers to examine the mechanical behavior of bioactive composites, and the interfacial interactions between the polymer and HAP crystals are addressed. The FTIR results confirmed that the two forms of HAP crystals are consistent in terms of the functional chemical groups. The wide angle X-ray diffraction study was performed to determine the crystallinity of the bioactive composites. It was observed that the crystallinty of HAP-filled PCL steadily increased as the filler concentration increased. Generally, HAP(2) has a particle size considerably smaller than HAP(1) and the composite derived had higher modulus than conventional HAP-filled polymers. This increase in modulus is attributed to better interfacial interaction. Bioresorbability tests performed on HAP particles found that the synthesized HAP had higher resorption rates. It is clear that the mechanical properties are influenced by the particle size and therefore by the processing method used.     

Enhancement of osteoblast gene expression by mechanically compatible porous Si-rich nanocomposite

Synthesis of a porous bioactive ceramic implant for load bearing applications is a challenging task in maxillofacial and orthopedic surgeries. A novel bioactive resorbable silica-calcium phosphate nanocomposite (SCPC) has recently been introduced as a potential bone graft. In the present study, we employed SCPC to develop a resorbable porous scaffold and analyzed the effects of composition and porosity on the mechanical properties. The ranges of compressive strength and modulus of elasticity of SCPC containing 32-56% porosity were 1.5-50 MPa and 0.14-2.1 GPa, respectively, which matched the corresponding values for trabecular bone. The compressive strength of dense SCPC was dependent on the Si content and acquired values (93-285 MPa) comparable to that of cortical bone. The superior mechanical properties of SCPC are attributed to the intricate interactions at the boundaries of the nanograins and to the homogenous distribution of hierarchical pore-structure throughout the material volume. X-ray computed tomography and mercury porosimetry analyses revealed high interconnectivity of the pores in the size range 3 nm to 650 microm. Quantitative real-time PCR analyses showed that neonatal rat calvarial osteoblasts attached to Si-rich SCPC expressed 5- and 26-fold higher osteocalcin mRNA levels compared to cells attached to ProOsteon hydroxyapatite disks and tissue culture polystyrene plates respectively, after four days in culture. Results of the present study strongly suggest that porous, bioactive resorbable SCPCs can serve as tissue engineering scaffolds for cell delivery to treat load-bearing bone defects in orthopedic and maxillofacial surgeries.     

Bioresorbable devices made of forged composites of hydroxyapatite (HA) particles and poly-L-lactide (PLLA): Part I. Basic characteristics

Compounds that had neither calcined nor sintered hydroxyapatite (u-HA) particles (particulate size 0.2-20 microns, averaging 3.0 microns, Ca/P = 1.69, and containing CO3(2-) uniformly distributed in a poly-L-lactide (PLLA, Mv: 400 KDa) matrix with a content of 20-50 wt% (with 10% increment) were reinforced into composites by a forging process, which was a unique compression molding, and were then machined on a lathe in order to produce practical radiopaque internal bone fixation devices having high mechanical strength which was maintained during bony union, total resorbability and bioactivity such as bone bonding capability and osteoconductivity. From the results of measurement of various mechanical properties, it was confirmed that the composites generally showed the highest mechanical strength among this type of reinforced bioceramic fibers or particles/bioresorbable polymer composite known to date. The bending strength (Sb) of about 270 MPa was far higher value than that for cortical bone, and the modulus (Eb) of 12 GPa was almost equivalent to that for cortical bone. In particular, the impact strength (Si) was extremely high at about two times the value (166 KJ/m2) of polycarbonate. The in vitro change in Sb, Mv (viscosity average molecular weight), Mw/Mn (molecular weight distribution) and crystallinity, and their relationship with each other was also examined by immersing samples in a phosphate buffer solution (PBS). An immediate decrease in the initial Mv could be found in composites with high u-HA contents (30-50 wt%), although a time-lag stage for degradation where the initial Mv hardly changes was apparent in cases of PLLA-only or in a composite with a low u-HA content (20 wt%). The Sb changed with corresponding decremental curves for the Mv and retained over 200 MPa for up to 24 weeks, the period of time necessary for full bony union, so that the composite satisfied initial mechanical strengths while maintaining them for as long as necessary for internal bone fixation devices. These results supported the idea that there is a difference in the degradation process such that PLLA alone required a period of time to achieve the possibility of hydrolysis into the inner side, whereas composites with high u-HA contents (30-50 wt%) immediately filled with water through to the inner side and were hydrolyzed homogeneously. Many hydroxyapatite crystals deposited and grew on the surface after 3-6 d and generously covered the surface with a fairly thick layer after 7 d of post-immersion in simulated body fluid (SBF) as evaluated by means of energy dispersive X-ray (EDX). This suggested the ability of the radiopaque composites to bond to bone. Since the composites were dense and had ultra-high strength, and the processability was so excellent, many kinds of fine and accurate screws, pins, plates, and other internal bone fixation devices for orthopedic, oral and maxillofacial, craniofacial, and plastic and reconstructive surgeries could be produced by machining treatment. These devices have potential applications for clinical use following the assessment of adaptation during in vivo studies.     

Effect of in vitro degradation of poly(D,L-lactide)/beta-tricalcium composite on its shape-memory properties

The in vitro degradation characteristic and shape-memory properties of poly(D,L-lactide) (PDLLA)/beta-tricalcium phosphate (beta-TCP) composites were investigated because of their wide application in biomedical fields. In this article, PDLLA and crystalline beta-TCP were compounded and interesting shape-memory behaviors of the composite were first investigated. Then, in vitro degradation of the PDLLA/beta-TCP composites with weight ratios of 1:1, 2:1, and 3:1 was performed in phosphate buffer saline solution (PBS) (154 mM, pH 7.4) at 37 degrees C. The effect of in vitro degradation time for PDLLA/beta-TCP composites on shape-memory properties was studied by scanning electron microscopy, differential scanning calorimetry, gel permeation chromatography, X-ray diffraction (XRD), and Fourier transform infrared spectroscopy (FTIR). The changes of structural morphology, glass transition temperature (T(g)), molecular weight, and weight loss of composites matrix and pH change of degradation medium indicated that shape-memory effects at different degradation time were nonlinearly influenced because of the breaking down of polymer chain and the formation of degradation products. Furthermore, the results from XRD and FTIR implied that the degradation products, for example, hydroxyapatite (HA), calcium hydrogen phosphate (CaHPO(4)), and calcium pyrophosphate (Ca(2)P(2)O(7)) phases also had some effects on shape-memory properties during the degradation.     

Autologous bone versus calcium-phosphate ceramics in treatment of experimental bone defects

Autologous bone grafting is currently considered the treatment of choice for correction of large bone defects. However, to avoid morbidity associated with autologous bone harvesting many artificial bone-substitute materials have been developed over the years. A new generation of resorbable materials is emerging, with promising results so far. In order to investigate the possibility to use one of these new materials as an alternative with better results than hydroxyapatite, an experimental study was performed. A new resorbable calcium phosphate particles and paste forms, the latter of which hardens in situ after application. In 28 sheep, a 3-cm segmental tibial defect was made and intramedullary fixed by an interlocking nail. Twelve weeks after defect filling, radiological, biomechanical, and histological examinations were performed. Mean radiographic and biomechanical tests results were compared with the Mann-Whitney test. Significance was set at p<0.05. Radiographically, the resorbable paste group performed better than all other groups. Biomechanical investigations showed a higher torsional stiffness (p=0.049) for the resorbable calcium-phosphate paste group in comparison with autologous bone. On histological examination, no adverse effects were observed in the calcium-phosphate groups. Resorption by osteoclasts was seen in the resorbable implants. In conclusion, the current study shows an advantageous radiological and mechanical outcome for resorbable calcium phosphates. This indicates that these new materials might be a potential alternative for autologous bone grafting in humans.     

Three body wear studies of five dental composites preconditioned in food simulating media

Progressive three body wear up to 30 min for five dental composites (Concise, Heliomolar, Occlusin, P-30, Profile, TPH) stored for 9 months at 37 degrees C in citrate, lactate and PBS buffers, 25 and 75% ethanol media, has been measured using a wear tester. Particle size of the filler and the storage media are found to play dominant roles in determining the extent of wear. Heliomolar, which is a microfilled composite, shows maximum wear whereas wear is least in composites containing filler particles of conventional and hybrid size such as P-30 (> 1 micron). The storage media is found to attack and degrade glass filler particles compared to composites having quartz fillers.     

Poly(epsilon-caprolactone-co-D,L-lactide) /silk fibroin composite materials: preparation and characterization

Poly(epsilon-caprolactone-co-D,L-lactide) copolymers with 10, 30, and 50% by weight of silk particles (size range: 5-250 microm) derived from Bombyx mori were blended in acetone solution. After evaporation of the solvent, the morphology, thermal behavior, and mechanical properties of the composites were examined. The composites were transparent and the silk fibroin particles were homogeneously distributed within the composite structure. The particles appeared as bright reflected images under the optical microscope, suggesting that they were in a crystalline state. DSC thermograms of the composites revealed that the glass transition of the matrix was at ca. -18 degrees C. Degradation of the silk fibroin occurred beyond 270 degrees C. The decomposition temperatures and degradation rate decreased with increasing silk fibroin content as revealed by TGA analysis. FTIR spectra of the composites showed absorption bands at 1730 and 1088 cm(-1) for the copolymer and at 3273 and 1617 cm(-1) for the silk fibroin. Although the characteristic lines of poly(epsilon-caprolactone-co-D,L-lactide) were independent of filler concentration. the absorption bands of the beta-sheet form of the silk fibroin increased slightly due to the interaction of silk fibroin with the copolymer.     

Bioresorbable composite bone paste using polysaccharide based nano hydroxyapatite

Aim of this study concerns to the development of bioresorbable composite materials for bone repair and regeneration. Despite nano hydroxyapatite (HA) has wide range of medical applications, particles mobilization and slow resorbable nature limits its use in certain applications particularly, periodontal and alveolar ridge augmentation. To enhance its usage, we have prepared HA composite bone paste with a natural polysaccharide, chitosan, using wet chemical method at low temperature. The prepared composites were analyzed by various physicochemical methods and suggesting that the nano HA crystallites are well intact with the chitosan macromolecules. FT-IR results are indicating the existence of hydroxyl and amide groups in addition to the characteristic peaks of nano HA in the composite paste. The physical nature of paste form implies that it would be highly beneficial for the particle immobilization upon implantation. In vitro physiological stability and solubility of the composite was performed in phosphate buffered saline under physiological condition and found that the rate of resorbability of composite was quite higher than nano HA. These findings suggest that the HA/chitosan composites may have a great impact on human health care systems as bioresorbable bone substitute.     

Analysis of apatite layers on glass-ceramic particulate using FTIR and FT-Raman spectroscopy

A nucleation and crystallization schedule was adapted to produce 40% crystalline Bioglass ceramic particulates. These particles were placed in a dynamic environment in a simulated physiologic solution (SBF-9) for time periods ranging from 10 min to 7 days. Fourier transform Raman spectroscopy (FT-Raman) and infrared spectroscopy (FTIR) were used to analyze the apatite layer formation on the particulates. FTIR determined that amorphous apatite formation took place within 2 h, with the appearance of crystalline apatite in 14 h. The vibrational frequencies obtained through FT-Raman were equivalent to those obtained using FTIR. These analyses showed that a fully crystallized apatite layer was present on the particulate after 3 days of exposure in SBF solution. These findings are consistent with those associated with amorphous Bioglass particles.     

Porous silicon-poly(ε-caprolactone) film composites: evaluation of drug release and degradation behavior

This work focuses on an evaluation of novel composites of porous silicon (pSi) with the biocompatible polymer ε-polycaprolactone (PCL) for drug delivery and tissue engineering applications. The degradation behavior of the composites in terms of their morphology along with the effect of pSi on polymer degradation was monitored. PSi particles loaded with the drug camptothecin (CPT) were physically embedded into PCL films formed from electrospun PCL fiber sheets. PSi/PCL composites revealed a release profile of CPT (monitored via fluorescence spectroscopy) in accordance with the Higuchi release model, with significantly lower burst release percentage compared to pSi microparticles alone. Degradation studies of the composites, using gravimetric analysis, differential scanning calorimetry (DSC), and field emission scanning electron microscopy (FESEM), carried out in phosphate-buffered saline (PBS) under simulated physiological conditions, indicated a modest mass loss (15%) over 5 weeks due to pSi dissolution and minor polymer hydrolysis. DSC results showed that, relative to PCL-only controls, pSi suppressed crystallization of the polymer film during PBS exposure. This suppression affects the evolution of surface morphology during this exposure that, in turn, influences the degradation behavior of the polymer. The implications of the above properties of these composites as a possible therapeutic device are discussed.     

In vitro apatite formation and its growth kinetics on hydroxyapatite/polyetheretherketone biocomposites

The formation of biologically equivalent carbonate-containing apatite on the surface of synthetic hydroxyapatite (HA) is an important step leading to good bone healing. In this study, HA-reinforced polyetheretherketone (PEEK) composites were prepared by homogeneous mixing of HA and PEEK powders, compaction, and pressureless sintering. The bioactivity of HA/PEEK composite with 10, 20, 30 and 40 vol% HA was evaluated by immersing the composite disks in the simulated body fluid (SBF) for up to 4 weeks. The surface of composite with 40 vol% HA was covered by a layer of bone-like apatite just after 3 days of immersion, while 10 vol% HA was covered only after 28 days. This apatite layer was characterized by SEM, thin film X-ray diffractometer, attenuated total reflectance-Fourier transform infrared spectrometer (FTIR)/FTIR. Introducing a concept called apatite-forming capacity of SBF, growth kinetics of the apatite layer on the surface of the composite disks was carried out. The growth rate constant increased with HA volume fraction of the composite, suggesting that the bioactivity of the HA/PEEK composite increases with increasing HA volume fraction in the composite.     

Bioactive composites consisting of PEEK and calcium silicate powders

Bioactive bone-repairing materials with mechanical properties analogous to those of natural bone can be obtained through the combination of bioactive ceramic fillers with organic polymers. Previously, we developed novel bioactive microspheres in a binary CaO-SiO2 system produced through a sol-gel process as filler for the fabrication of composites. In this study, we fabricate bioactive composites in which polyetheretherketone is reinforced with 0-50 vol% 30CaO x 70SiO2 (CS) microspheres. The prepared composites reinforced with CS particles form hydroxyapatite on their surfaces in simulated body fluid. The induction periods of hydroxyapatite formation on the composites decrease with increasing amount of CS particles. The mechanical properties of the composites are evaluated by three-point bending test. The composites reinforced with 20 vol% CS particles show 123.5 MPa and 6.43 GPa in bending strength and Young's modulus, respectively.