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Calcium phosphate (Ca,P) precipitation behavior on the surface of two bioactive glasses and four bioactive glass composites--two with hydroxylapatite (Ca10(PO4)6 (OH)2) and two with rhenanite (CaNaPO4)--were studied in simulated body fluid (SBF) and in Tris-Buffer at 5, 8, 16, 24, 48, 72, and 144 h. The weight loss of the materials was measured and the amount of precipitation was estimated using scanning electron microscopy with electrochemical detection (SEM-EDX) analysis. The test was repeated for one glass and its respective rhenanite composite every 3 h until 60 h and thereafter every 10 h until 150 h in SBF. Atomic absorption spectroscopy, spectrophotometry, SEM-EDX analysis, and pH measurements were performed on these samples. It is shown that in vitro the composite materials have a higher capacity for Ca,P precipitation than the glasses. Weight losses of the materials correlate well with their composition. Both the glass and Ca,P phases influence the precipitation mechanism and rate. Precipitation begins preferably from the glass phase. Ca,P particles clearly influence the time of onset and rate of precipitation. Cross-sectional EDX analysis of the samples revealed an absence of a clear Si-rich layer in glass A0B0 (SiO2 53.9 mol %, Na2O 27.5, CaO 12.4, P2O5 6.2, Al2O3 0.0 and B2O3 0.0) composites. This was attributed to the presence of extra calcium and phosphate ions on the surface of the material. The ion-concentration and pH change curves offered insight into the mechanism of precipitation. A connection was established between SEM-EDX results and the release curves. Formation of an Si,Ca,Na film was observed that seemed to initiate the Ca,P precipitation.(ABSTRACT TRUNCATED AT 250 WORDS)
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PMID:Dissolution and scanning electron microscopic studies of Ca,P particle-containing bioactive glasses. 824 37

Bond coats for plasma-sprayed hydroxyapatite (HAp) coatings on Ti-6A1-4V hip endoprotheses are being developed for improved in vivo performance. Bond coat powders consisting of (i) CaO-stabilized zirconia, (ii) a eutectic composition of titania and non-stabilized zirconia, and (iii) titania were applied by atmospheric plasma spraying (APS) to Ti-6A1-4V-coupons and 100 microm-thick Ti-6A1-4V foils. Subsequently, a thick layer of HAp was sprayed onto the thin bond coats. Peel tests on Ti-6A1-4V foil/bond coat/HAp top coat assemblies revealed that titania and titania/ zirconia bond coats increased the peel adhesion strength in a statistically significant way from 22 N m(-1) (HAp without a bond coat) to >42 and 32 N m(-1), respectively. Microstructural investigations by SEM on cross-sections of coatings leached in simulated body fluid for up to 28 days led to the conclusion that the chemically very stable bond coats act as an improved chemical barrier against in vivo release of metal ions from the implant, as well as an improved adhesive bond by development of very thin well-adhering reaction layers, presumbly composed of perovskite, calcium dititanate, and/or calcium zirconate.
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PMID:Development of plasma-sprayed bioceramic coatings with bond coats based on titania and zirconia. 979 27

Previous work has shown that small additions of a phosphate glass (CaO-P2O5) can significantly enhance the sinterability and strength of hydroxyapatite. However, there are no quantitative phase analyses available for these materials which would provide indicators of biocompatibility and resorbability. Similarly, there is little information available about the mechanical properties, especially with high glass additions. In this study, the effects of sintering hydroxyapatite with phosphate glass additions of 2.5, 5, 10, 25, and 50 wt.% are quantified. Each composition was sintered over a range of temperatures, and quantitative phase analysis was carried out using XRD. In addition, the microstructures were studied using RLOM and SEM, and mechanical properties (Vickers hardness, KIC, and MOR) measured. These results may be used to indicate which compositions and processing conditions may provide materials suitable for use in hard tissue replacement. Composites containing up to 10 wt.% glass additions formed dense HA/TCP composite materials possessing flexural strength and fracture toughness values up to 200% those of pure HA. The HA/TCP ratio was strongly dependent on the percentage glass addition. Higher glass additions resulted in composites containing beta-TCP together with large amounts of alpha- or beta-calcium pyrophosphate, and having similar mechanical strengths to pure HA.
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PMID:A quantitative study of the sintering and mechanical properties of hydroxyapatite/phosphate glass composites. 985 84

CaO-P(2)O(5) glasses with additions of MgO and CaF(2) were used as a sintering aid of hydroxyapatite, and glass-reinforced hydroxyapatite composites obtained. Glasses promoted significant changes in the microstructure of the composites, namely with the formation of tricalcium phosphate secondary phases, beta and alpha-TCP. Quantitative phase analysis was performed by the Rietveld method using General Structure Analysis Software. Grain size measurements were carried out on SEM photomicrographs, using a planimetric procedure according to ASTM E 112-88. Flexural bending strength was determined from concentric ring-on-ring testing. Flexural bending strength (FBS) of glass-reinforced hydroxyapatite composites was found to be about twice or three times higher than that of unreinforced hydroxyapatite and tended to depend more on porosity and beta and alpha-TCP secondary phases, rather than on grain size. Traces of alpha-tricalcium phosphate significantly enhanced the strength of the composites. Using the rule of mixtures to estimate the zero porosity bending strength, the Duckworth-Knudsen model applied to the composites gave a porosity correction factor, b, with a value of 4.02. Weibull statistics were also used to analyze biaxial strength data and the level of reinforcement obtained by comparing failure probability for the composites and for the unreinforced hydroxyapatite. Lower activation energies for grain growth were observed for the composites compared to unreinforced hydroxyapatite, which should be attributed to the presence of a liquid glassy phase that promotes atomic diffusion during the sintering process.
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PMID:Glass-reinforced hydroxyapatite composites: secondary phase proportions and densification effects on biaxial bending strength. 1049 Jun 90

The aim of this work has been to test the biocompatibility of four bioactive, gel derived glass-ceramic materials of CaO-PO2-SiO2 system, modified by addition of boron, aluminum and magnesium compounds. We have examined the growth, collagen synthesis, adhesion and morphology of NRK rat fibroblasts cultured in direct and indirect contact with biomaterials. The growth of cells cultures has been quantified by two methods: [3H]thymidine incorporation and direct counting of cells. The level of collagen synthesis has been used as a parameter describing metabolic activity of cells. Cellular morphology has been assessed following 24 h and 4 days of culturing cells on biomaterials by using SEM and confocal microscopy, respectively. Additionally, in order to obtain information about the attachment of cells to substratum the presence of focal contacts has been examined. The results of all the experiments have demonstrated that none of the materials under study significantly altered cellular functions that were tested. This indicates that additions of MgO, Al2O3 and B2O3 have not induced cytotoxicity of the materials under study. This qualifies them for further in vivo experiments.
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PMID:Evaluation of biocompatibility of apatite-wollastonite ceramics in fibroblast cultures. 1097 73

Hydrothermal method was used to prepare the hydroxyapatite (HA) coating on CaO-SiO2-B2O3-Na2O glass. The phase composition, morphology and microstructure of HA coated glass composites were analyzed using XRD, EPMA, FT-IR and SEM techniques. It revealed that HA coating possessed a porous gradient construction; HA coating was tightly bonded with the glass substrate by the interface layer. During the formation of HA coating, the hydrated silica produced by the corrosion of glass substrate in the hydrothermal solution provided favorable sites for apatite nucleation. With the dissolving of HA powder and the growth of apatite small crystallites, Ca+, PO(4 (3-)) ions would precipitate on the surface of glass to form the HA coating. Silicon element released from glass reacted with calcium produced by the dissolution of HA to form the tight reaction layer. HA coating is formed by the mechanism of dissolving-ions immigrating-precipitating pattern.
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PMID:Morphology and formation mechanism of hydroxyapatite coating by hydrothermal method on CaO-SiO2-B2O3-Na2O glass. 1120 48

This paper has studied the dissolution behavior of the plasma sprayed and electrochemically prepared hydroxyapatite(HA) biocoatings in the simulated body fluid. XRD and SEM show that the plasma sprayed coating and post-heat treated HA coatings are more soluble, and CaO and alpha-TCP in the coatings gradually disappear and CaCO3 forms during the immersion. The composition of the electrocrystallized and alkaline-treated HA coatings is basically unchanged, and the coatings are more stable in the simulated body fluid.
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PMID:[In vitro dissolution study on the hydroxyapatite biocoatings]. 1121 16

Nonwoven sheets of bioactive fibers were produced using a sol-gel process. A high velocity spray process was used to prepare fibers of two compositions in the SiO(2)-CaO-P(2)O(5) ternary system. Both discontinuous fibers and dispersed fibers were evaluated. Viscosity and pH of the sol were the two primary processing variables studied. The formation of hydroxy carbonate apatite (HCA) on the surface of the fibers was used to evaluate the kinetics of the bioactivity in a simulated body fluid (SBF). Diffuse reflection infrared fourier transform spectroscopic (DRIFTS) analysis confirmed the presence of HCA (P-O). A homogenous layer of HCA, as observed with SEM (scanning electron microscopy), typically formed after 3-h immersion in the SBF. The concentration of HCA formed was greater for samples richer in silica. The new bioactive fiber sheets produced by this process are chemically more stable than powders or monoliths prepared from similar precursors. Potential applications are as scaffold for both mineralized and nonmineralized structural tissues.
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PMID:A sol-gel derived bioactive fibrous mesh. 1128 74

This paper evaluates the behavior of hydroxyapatite (HAP) coated and noncoated Ti6Al4V implants in dog tibia after 3 and 5 months implantation. HPA-coated implants were obtained by plasma spraying. XRD, SEM, and EPMA were employed to estimate the coating characteristics and their behavior in vivo. Investigation of material characteristics showed that the as-received coatings consisted mainly of amorphism and HAP phase. Other phases such as TCP and CaO were identified due to thermal changes of HAP particles in plasma flame. SEM micrographs showed a typical microstructure of plasma-sprayed coating. The as-received coating was formed by well-melted pancake-like splats that lead to a dense coating with a rough surface. Lamellar structure, micropores, and microcracks, observed inside the coating, are characteristic of plasma spraying. Push-out tests revealed that HAP coating had a significant promotion of interfacial shear strength. The shear strength between bone and HAP-coated implants was much higher than that between bone and noncoated implants due to the different bone-implant interfaces formed after implantation. SEM observation revealed a direct attachment between HAP coating and newly formed bone. However, noncoated implants were separated from newly formed bone by fibrous tissues. Ti ions were found to be released into the surrounding environment after long time immersion in body fluid, and thus caused low shear strength. Prolongation of implantation time had different effects on shear strength. It improved the shear strength between HAP-coated implant and newly formed bone. However, it had little effect on that between noncoated implant and surrounding tissues.
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PMID:Mechanical and histological evaluations of hydroxyapatite-coated and noncoated Ti6Al4V implants in tibia bone. 1130 86

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.
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PMID:In vitro bioactivity of S520 glass fibers and initial assessment of osteoblast attachment. 1451 88


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