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EN
Biohybrids consisting of gelatin (G) and calcium phosphate silicate/wollastonite (CPS/W) have not been prepared so far. In this work our results are focused on the possibility of obtaining G-CPS/W bioactive hybrids in vitro. XRD, FTIR, SEM/EDS techniques were employed to characterize the synthesized hybrid materials. FTIR shows that before immersion in 1.5 SBF the “red shift” of COO- band for pure G is observed. The presence of this bond could be attributed to the formation of COO-Ca2+ via non-biomimetic route. After immersion in 1.5 SBF, FTIR shows the presence of A- and B-type carbonate containing hydroxyapatite (A/B-CO3HA). ESD and FTIR show that small amount of calcite (CaCO3) are present after in vitro test in 1.5 SBF for 3 days. XRD reveals that CO3HA and small amounts of CaCO3 can be detected after in vitro test. SEM results obtained for immersed samples show that hydroxyapatite (HA) particles fully covered the surface of the hybrids by a layer composed of spherulites. At higher magnification, very small elongated crystallites could be observed. [...]
EN
The 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. [...]
EN
In this work we present experimental results about synthesis, structure evolution and in vitro bioactivity of new calcium phosphate silicate/wollastonite (CPS/W) glass-ceramics. The samples obtained were synthesized via polystep sol-gel process with different Ca/P+Si molar ratio (R). The structure of the materials obtained was studied by XRD, FTIR spectroscopy and SEM. XRD showed the presence of Ca15(PO4)2(SiO4)6, β-CaSiO3 and α-CaSiO3 for the sample with R=1.89 after thermal treatment at 1200°C/2h. The XRD results are in good agreement with FTIR analysis. SEM denotes that apatite formation can be observed after soaking in simulated body fluid (SBF). [...]
EN
In this work we present our experimental results on synthesis, structure evolution and in vitro bioactivity assessment of new gelatin/silicocarnotite hybrid materials. The hybrids were obtained by diluting gelatin (G) and silicocarnotite (S) ceramic powder with G:S ratios of 75:25 and 25:75 wt.% in hot (40°C) water. The hybrids were characterized using XRD, FTIR, SEM/EDS and XPS. FTIR depicts that the “red shift” of amide I and COO− could be attributed to the fact that the gelatin prefers to chelate Ca2+ from S. The growth of calcium phosphates on the surface of the hybrids synthesized and then immersed in 1.5 SBF for 3 days was studied by using of FTIR, XRD and SEM/EDS. According to FTIR results, after an immersion of 3 days, A and B-type CO3HA can be observed on the surface. XRD results indicate the presence of hydroxyapatite with well defined crystallinity. SEM/EDS of the precipitated layers show the presence of CO3HA and amorphous calcium phosphate on the surface of samples with different G/S content when immersed in 1.5 SBF. XPS of the G/S hybrid with 25:75 wt.% proved the presence of Ca-deficient hydroxyapatite after an in vitro test for 3 days.
EN
In the present work Polyurethane (PU)/Bioglass (BG) composite materials were synthesized with different content of BG (10 and 20 mol.%) as filler. The 85S Bioglass was synthesized via polystep sol-gel method. The chemical composition of BG is 85SiO2-10CaO-5P2O5 (wt.%). The synthesis of PU was carried out by a two-step polyaddition reaction. The 85S BG was added in situ during the polymerization reaction. In vitro bioactivity of the prepared composites was examined in the presence of 1.5 SBF for 7 days in static conditions. The structure of synthesized PU/BG composites before and after in vitro test was determined by XRD, FTIR and SEM. XRD of the samples before in vitro test proved that the phase of γCa2P2O7 in the PU/20BG is visible. FTIR revealed the presence of urethane bond between OH-(from BG) and NCO groups (from PU). Based on FTIR results after in vitro test in 1.5 SBF solutions, A/B-carbonate containing hydroxyapatite (CO3HA) was formed. XRD proved that HA was formed on the surface of the samples, but Ca2P2O7 does not undergo any changes in the 1.5 SBF solution. SEM depicted the nano-HA agglomerated in spherical particles after immersion in 1.5 SBF for 7 days.
EN
The silicocarnotite, as an inorganic part of the coatings, has been synthesized using a polystep sol-gel method. The chemical composition of the prepared silicocarnotite sol is described as 58.12 CaO, 29.42 P2O5, 12.45 SiO2 (wt%), where Ca/P+Si = 1,67. The acid soluble type I collagen, as an organic part of the obtained coatings, was mixed with silicocarnotite powder in a weight ratio of 25:75 and 75:25 weight ratio without cross-linkage. The acidity of the obtained mixture was readjust with 25% NH4OH to pH = 9.0. The mixture was then dried at 37°C for 12 h. The growth of B-type carbonate containing hydroxyapatite (B-type CO3HA) in which CO3 2+→PO4 3− on the surface of collagen/silicocarnotite coatings soaked in 1.5 simulated body fluid (1.5 SBF) was observed. The nucleation of B-type CO3HA was estimated on the obtained coatings after 3 days immersion in 1.5 SBF. The negatively charged carboxylate groups from the collagen surface may be responsible for the HA deposition. This was confirmed by the “red shift” of carboxylate groups of collagen molecules in the FTIR spectra. After soaking in 1.5 SBF, the morphology of prepared coatings and HA formation was observed by SEM.
EN
The 70SiO2-30CaO (wt.%) sol-gel glasses doped with 1, 3 and 5 NbF5 (wt.%) were prepared via polystep sol-gel route. The synthesized glasses were characterized by XRD, FTIR and SEM. Changes in 1.5 SBF solutions were measured by ICP-AES. XRD of the glasses stabilized at 700°C for 6 hours proved the presence of niocalite. FTIR was consistent with XRD data. The in vitro bioactivity study of all glasses prepared were carried out by soaking in 1.5 simulated body fluid (1.5 SBF) at 37°C for 6 and 12 days in static conditions. The FTIR reveals the formation of A-type and B-type carbonate containing hydroxyapatite (CO3HA) layer. Changes in 1.5 SBF solutions, after 6 days of soaking, show that the Ca concentration increased significantly, compared to the initial Ca content in the 1.5 SBF solution before in vitro test. After 12 days of immersion, the Ca concentration decreased, i.e., the formation of HA phase consumed Ca from 1.5 SBF solution. For all soaking times, the concentration of P is much lower than that the used 1.5 SBF. Based on these results we suggest that Ca and P play an active role in the future of the glasses. SEM depicts that the different morphology of hydroxyapatite can be formed as a function of soaking time.
EN
Ceramics, with basic composition based on the CaO-SiO2-P2O5-MgO system with different Ca+ Mg/P+Si molar ratio (R), were prepared via polystep sol-gel technique. The structure of the obtained ceramic materials has been studied by XRD, FTIR spectroscopy, and SEM. X-ray diffraction showed the presence of akermanite and HA for the sample with R = 1.68 and Mg substituted β-TCP and silicocarnotite for the sample with R = 2.16, after thermal treatment at 1200°C/2 h. The obtained results are in good agreement with FTIR. In vitro test for bioactivity in static condition proved that the carbonate containing hydroxyapatite (CO3HA) can be formed on the surface of the synthesized samples. CO3HA consisted of both A- and B-type CO 32− ions. SEM micrographs depicted different forms of HA particles, precipitated on the surface after soaking in 1.5 simulated body fluid (SBF). [...]
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