Jana Kozánková

Fluoroapatite - material for medicine, Growth, morphology and thermoanalytical properties

Fluoroapatite containing glass-ceramics were prepared from Li2O-CaO-CaF2-P2O5-SiO2 system. The glass was melted at 1480°C for 1 h. The object of observation was the preparing crystal phase of fluoroapatite in amorphous glass matrix. The morphology of lithium disilicate glass-ceramics was studied by SEM. The crystal growth and thermal properties of fluoroapatite were studied by X-ray diffraction and DTA. The more the content of P2O5, the more the presence of fluoroapatite particles. SEM investigation clearly indicated the phase separation and formation of a primary crystalline phase of fluoroapatite in the studied glass-ceramics. DTA curves of the fluoroapatite samples exhibit exothermic effects in the temperature range 337-694°C depending on the composition of the materials. The position of exothermic peak for lithium disilicate on DTA curves moves with increasing specific surfacetowards lower temperatures which points on its preferential surface crystallization. As far as physical qualities are concerned, mainly color and gloss, the best qualities of all observed materials belong to glass-ceramics with 10% P2O5.

Synthesis of poly(vinyl alcohol) — hydroxyapatite composites and characterization of their bioactivity

A series of poly(vinyl alcohol) membranes reinforced with hydroxyapatite in various weight percent — 0%, 10%, 20%, 30%, 40% and 50% were prepared. Hydroxyapatite was prepared by a sol-gel procedure using diammonium hydrogen phosphate and calcium nitrate tetrahydrate as starting materials in an alkaline aqueous environment and then mixed with a solution of poly(vinyl alcohol), which was prepared by dissolving it in water at 85°C.The different mixtures were cast in a mould and evaporated for 7 days at a temperature of 30°C to obtain 1 mm thin membranes. FTIR spectroscopy was used to identify the different functional groups in the composites. The surface morphology was examined using a scanning electron microscope. In vitro bioactivity tests in Simulated Blood Fluid were performed for up to 28 days, especially for the membrane containing 50 wt.% HA. SEM was used to characterise the surface microstructure of biocomposite membranes before and after soaking in SBF. It was observed that the formation of clusters in membranes increases with increasing amount of HA. The clusters are formed due to agglomeration and crystal growth of HA particles during drying of the membranes. The in vitro bioactivity was found to increase with soaking time of biocomposite materials in simulated blood fluid.Graphical abstract

Characterization of cordierite-mullite ceramics prepared from natural raw materials

Abstract Series of six cordierite-mullite ceramics were synthesized via solid state reaction at various temperatures from 1250 °C for pure cordierite to 1500 °C for pure mullite. Then the samples were submitted to the test of thermal shock resistance based on cycling heating-quenching procedure. X-ray diffraction (XRD), Scanning electron microscopy (SEM) and Mercury intrusion porosimeter (MIP) have been used to characterize the samples before and after cycling heating-quenching method. Sample 6 was broken after 35 heating-quenching cycles, while the five other reminded stable. The refractoriness of samples is found to be higher than that of commercial ones. XRD shows that heating-quenching procedure has led to crystallization of cordierite and mullite phases. Apart from sample 6, the pore structure is stable with slight consolidation. The microstructure images confirm the results of XRD and MIP showing crack in sample 6 only, but compact and larger particles resulting from crystal growth in other samples due to the repeated action of heating.

Polyvinylpyrrolidone thin film pyrolysis as accessed by the real-time optical transmission measurements

Present results reveal basic features of the optical transmission thermo-analytical method in its employment to investigate the oxidative pyrolysis of supported thin polyvinylpyrrolidone films. The OT curves naturally vary in shapes and positions on the time/temperature scales, respective to the examined rate of sample heating, to the wavelengths of radiation as well as to the film thickness. Recorded OT curves exhibit characteristic shapes with well-expressed OT minima. The temperatures at which the OT minima appear are in a linear relationship with heating rates of samples, at a frequency of radiation as well as a film thickness kept constant. Similarly, the OT values at which the OT minima appear are in a linear relationship with film thickness, at a frequency of the radiation and sample heating rate unchanged.

Characterisation of the surface structure and bioactivity of glass and glass ceramics using surface topography

AbstractThe present paper reports the results of the relationship between the surface topography, microstructure and the in vitro bioactivity of samples with and without fluorapatite content in simulated body fluid. Glasses and glass ceramics belonging to the Li2O-SiO2-CaO-P2O5-CaF2 system were prepared by using conventional melting technique following by heat treatment to obtain glass ceramics. This current study demonstrates the benefits of combining two microscopic methods for better investigation of the surface structure. The formation of apatite layer on the surface and the increase in surface roughness proved that the glasses and glass ceramics with bioactive fluorapatite content could satisfy to the requirements for biomaterial applications. The results also showed that the roughness of apatite layer formed after immersion in body fluid on the surface of glasses with fluorapatite was more pronounced than that of equivalent glass ceramic samples cured under the same conditions.

Preliminary comparison static and dynamic in vitro test of bioactivity of glass-ceramics

The bioactivity of glass ceramics with different amount of fluorapatite expressed as P2O5 content has been tested in vitro in static and dynamic regime. The paper reports the complete results of bioactivity test of glass-ceramics in static regime. XRD, SEM, and microprobe analysis were used to characterise the sample as well as to detect the presence of new phase onto the surface. The bioactivity, as demonstrated by the formation of new apatite layer, depends on P2O5 content. In static regime, the layer of hydroxyapatite develops by periodical deposition of spherical apatite bullet. In the dynamic test regime, the microstructure of apatite layer formed on the surface of sample is porous and grows as a result of continual reaction between the layer and fluid.