Phase composition, crystal structure and morphology of biological hydroxyapatite (BHAp) extracted from human mandible bone, and carbonated hydroxyapatite (CHAp), synthesized by the chemical precipitation method, were studied by x-ray powder diffraction (XRD), Fourier transform infrared (FTIR) and Raman (R) spectroscopy techniques, combined with transmission electron microscopy (TEM). Structural and microstructural parameters were determined through Rietveld refinement of recorded XRD data, performed using the FullProf computing program, and TEM. Microstructural analysis shows anisotropic extension along the [00l] crystallographic direction (i.e. elongated crystallites shape) of both investigated samples. The average crystallite sizes of 10 and 8 nm were estimated for BHAp and CHAp, respectively. The FTIR and R spectroscopy studies show that carbonate ions substitute both phosphate and hydroxyl ions in the crystal structure of BHAp as well as in CHAp, indicating that both of them are mixed AB-type of CHAp. The thermal behaviour and carbonate content were analysed using thermogravimetric and differential thermal analysis. The carbonate content of about 1 wt.% and phase transition, at near 790 °C, from HAp to β-tricalcium phosphate were determined in both samples. The quality of synthesized CHAp powder, particularly, the particle size distribution and uniformity of morphology, was analysed by a particle size analyser based on laser diffraction and field emission scanning electron microscopy, respectively. These data were used to discuss similarity between natural and synthetic CHAp. Good correlation between the unit cell parameters, average crystallite size, morphology, carbonate content and crystallographic positions of carbonate ions in natural and synthetic HAp samples was found.
3D network configurations of copper(II) oxide/titanate nanobelt (CuO/TiNBs) and copper/titanate nanobelt (Cu/TiNBs) were formed using a two-step polyelectrolyte-assisted synthesis and assembly approach. The photoactivity of the TiNB/CuO and Cu/TiNB composite networks is significantly enhanced as compared to the activity of 3D structures formed of pristine TiNB. An efficient, UV-vis-light-induced electron transfer at the two-component interface achieved by the intimate coupling of TiNB with p-type semiconducting CuO and plasmonic Cu nanoparticles in composite heterostructures facilitates control over the system's exciton dynamics, which results in highly efficient UV-vis photocatalytic performance of heterostructures. The superior photocatalytic activity of the metal and semiconductor/semiconductor nanocomposite structures in the visible region is discussed, highlighting the role of interfacial electron-charge transfer (IFCT) in semiconductor-semiconductor (CuO/TiNB) and surface plasmon resonance (SPR) of Cu nanoparticles in metal-semiconductor heterostructures.
A series of cobalt‐exchanged hydroxyapatite (CoHAp) powders with different Ca/Co ratios and nominal unit‐cell contents Ca10−xCox(PO4)6(OH)2, x = 0, 0.5, 1.0, 1.5 and 2.0, were synthesized by hydrothermal treatment of a precipitate at 473 K for 8 h. Based on ICP (inductively coupled plasma) emission spectroscopy analysis, it was established that the maximum amount of cobalt incorporation saturated at ∼12 at.% under these conditions. The effects of cobalt content on the CoHAp powders were investigated using ICP emission spectroscopy, particle size analysis, transmission electron microscopy (TEM) and high‐resolution transmission electron microscopy (HRTEM) analyses as well as X‐ray powder diffraction (XRPD) including Rietveld analysis. According to XRPD, all the materials are single‐phase HAp and CoHAp of low crystallinity. Rietveld analysis shows that Co enrichment causes the c cell parameter to decrease at a faster rate than the a cell parameter. A microstructural analysis showed anisotropic X‐ray line broadening due to crystallite size reduction. In CoHAp there is significant crystal elongation in [001], and the average size decreases with increasing cobalt content. The crystallite morphology transforms from rod‐like for the pure HAp to lamellae at the highest degree of Co substitution. The results of Rietveld refinement (symmetry, size and morphology of the crystallites) were confirmed by TEM and HRTEM analysis.
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