The present work was focused on the synthesis and characterization of hydroxyapatite doped with low concentrations of zinc (Zn:HAp) (0.01 < xZn < 0.05). The incorporation of low concentrations of Zn2+ ions in the hydroxyapatite (HAp) structure was achieved by co-precipitation method. The physico-chemical properties of the samples were characterized by X-ray Diffraction (XRD), Fourier Transform Infrared Spectroscopy (FTIR), X-ray photoelectron spectroscopy (XPS), Scanning Electron Microscopy (SEM), zeta-potential, and DLS and N2-BET measurements. The results obtained by XRD and FTIR studies demonstrated that doping hydroxyapatite with low concentrations of zinc leads to the formation of a hexagonal structure with lattice parameters characteristic to hydroxyapatite. The XRD studies have also shown that the crystallite size and lattice parameters of the unit cell depend on the substitutions of Ca2+ with Zn2+ in the apatitic structure. Moreover, the FTIR analysis revealed that the water content increases with the increase of zinc concentration. Furthermore, the Energy Dispersive X-ray Analysis (EDAX) and XPS analyses showed that the elements Ca, P, O, and Zn were found in all the Zn:HAp samples suggesting that the synthesized materials were zinc doped hydroxyapatite, Ca10−xZnx(PO4)6(OH), with 0.01 ≤ xZn ≤ 0.05. Antimicrobial assays on Staphylococcus aureus and Escherichia coli bacterial strains and HepG2 cell viability assay were carried out.
The present study is focused on the synthesis, characterization and antifungal evaluation of zinc-doped hydroxyapatite (Zn:HAp) coatings. The Zn:HAp coatings were deposited on a pure Si (Zn:HAp_Si) and Ti (Zn:HAp_Ti) substrate by a sol-gel dip coating method using a zinc-doped hydroxyapatite nanogel. The nature of the crystal phase was determined by X-ray diffraction (XRD). The crystalline phase of the prepared Zn:HAp composite was assigned to hexagonal hydroxyapatite in the P63/m space group. The colloidal properties of the resulting Zn:HAp (xZn = 0.1) nanogel were analyzed by Dynamic Light Scattering (DLS) and zeta potential. Scanning Electron Microscopy (SEM) was used to investigate the morphology of the zinc-doped hydroxyapatite (Zn:HAp) nanogel composite and Zn:HAp coatings. The elements Ca, P, O and Zn were found in the Zn:HAp composite. According to the EDX results, the degree of Zn substitution in the structure of Zn:HAp composite was 1.67 wt%. Moreover, the antifungal activity of Zn:HAp_Si and Zn:HAp_Ti against Candida albicans (C. albicans) was evaluated. A decrease in the number of surviving cells was not observed under dark conditions, whereas under daylight and UV light illumination a major decrease in the number of surviving cells was observed.
Antibacterial cerium-doped hydroxyapatite (Ce-HAp) layers have been researched sparingly in recent years. The Ce-HAp powder, Ca10−xCex(PO4)6(OH)2 with xCe = 0.05, was obtained by an adapted chemical co-precipitation method at room temperature. The target was prepared using the Ce-HAp (xCe = 0.05) powder sintered in air at 600 °C. The coatings on the Ti substrate were generated in plasma using a radio frequency (RF) magnetron sputtering discharge in an Ar gas flow in a single run. To collect the most complete information regarding the antimicrobial activity of cerium-doped hydroxyapatite with xCe = 0.05, (5Ce-HAp), antimicrobial studies were carried out both on the final suspensions and on the coated surfaces. The target was tested using ultrasound measurement, transmission electron microscopy (TEM), scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR), glow-discharge optical emission spectroscopy (GDOES), and X-ray photoelectron spectroscopy (XPS). The present study exhibited for the first time results of the homogeneous coatings of hydroxyapatite doped with cerium using a radio frequency magnetron sputtering technique. In addition, this study highlighted for the first time the stability of the cerium-doped hydroxyapatite gels used in the creation of the coating. Ultrasound measurements on the concentrated suspension of 5Ce-HAp showed a good stability compared to double distilled, water which was chosen as the reference fluid. Particles with spherical shape were observed by both TEM and SEM analysis. The broadening of the IR bands in the IR spectrum of the 5Ce-HAp film in comparison with the IR spectrum of the precursor target indicate the formation of interlinked bonds into the layer bulk. XPS analysis revealed that the mixture of Ce3+ and Ce4+ ions in the hydroxyapatite (HAp) structure of the coatings could be due to the deposition process. The surface of 5Ce-HAp coatings was homogenous with particles having a spherical shape. A uniform distribution of all the constituent elements on the surface the 5Ce-HAp layer was revealed. The antimicrobial assays proved that both 5Ce-HAp suspensions and 5Ce-HAp coatings effectively inhibited the development of colony forming units (CFU) for all the tested microbial strains. Moreover, the antimicrobial assays emphasized that the 5Ce-HAp suspensions had a biocide effect against Escherichia coli (E. coli) and Candida albicans (C. albicans) microbial strains after 72 h of incubation.
The main objective of this paper is to develop silver-doped hydroxyapatite suspensions (HApAg) with different concentrations of silver (xAg = 0.05 and xAg = 0.2) in order to obtain uniform and homogenous layers by spin-coating procedure. The colloidal properties of HApAg suspensions are evaluated by dynamic light scattering (DLS) analysis, ζ-potential (ZP), and ultrasound measurements. The ultrasound studies show that the HApAg20 sample revealed better stability than the HApAg5 sample. The structural and morphological analysis on suspensions and thin layers is also conducted. It is observed that the particles of the two samples have a similar shape and are uniform. The layers obtained present a homogeneous appearance of the surface without evidence of cracks or interruption of the coatings. The in vitro antifungal studies conducted on the two thin layers at two different time intervals (24 and 48 h) show that both HApAg5 (xAg = 0.05) and HApAg20 (xAg = 0.05) nanoparticles suspensions and composite layers inhibit the development of colony forming units (CFU) even after 24 h of incubation comparative to the control, represented by the Candida albicans (C. albicans) culture in a proper medium. The fungicidal effect was evident after 48 h of incubation in the case of both HApAg20 nanoparticles suspensions and composite layers.
The present study demonstrates the effectiveness of hydroxyapatite nanopowders in the adsorption of zinc in aqueous solutions. The synthesized hydroxyapatites before (HAp) and after the adsorption of zinc (at a concentration of 50 mg/L) in solution (HApD) were characterized using X-ray diffraction (XRD), and scanning and transmission electron microscopy (SEM and TEM, respectively). The effectiveness of hydroxyapatite nanopowders in the adsorption of zinc in aqueous solutions was stressed out through ultrasonic measurements. Both Langmuir and Freundlich models properly fitted on a wide range of concentration the equilibrium adsorption isotherms, allowing us to precisely quantify the affinity of zinc to hydroxyapatite nanopowders and to probe the efficacy of hydroxyapatite in removal of zinc ions from aqueous solutions in ultrasonic conditions.
In this study, we develop chitosan–hydroxyapatite (CS–HAp) composite layers that were deposited on Si substrates in radio frequency (RF) magnetron sputtering discharge in argon gas. The composition and structure of CS–HAp composite layers were investigated by analytical techniques, such as Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), metallographic microscopy (MM), and atomic force microscopy (AFM). On the other hand, in the present study the second order derivative of FT-IR–ATR spectra, for compositional analyses of CS–HAp, were used. The SEM, MM, and AFM data have shown the formation of CS–HAp composite layers. The surface of CS–HAp composite layers showed uniform growth (at an Ar gas working pressure of p = 2 × 10−3 mbar). The surface of the CS–HAp composites coatings became more nanostructured, becoming granular as the gas pressure increased from 5 × 10−3 to 1.2 × 10−2 mbar. However, our studies revealed that the surface morphology of the CS–HAp composite layers varies with the Ar gas working pressure. At the same time, optical properties are slightly influenced by Ar pressure. Their unique physicochemical properties make them suitable for various applications in the biomedical field, if we consider the already proven antimicrobial properties of chitosan. The antifungal properties and the capacity of the CS–HAp composite layers to inhibit the development of fungal biofilms were also demonstrated using the Candida albicans ATCC 10231 (C. albicans) fungal strain.