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.
12 February 2010 in Journal of Applied Crystallography
Geopolymeric binders (GB) were produced using fly ash (FA) and electric arc furnace slag (EAFS). The slag has been added in the range of 0–40%. The effects of slag content on the strength, microstructure and thermal resistance were evaluated. It was found that the amount of EAFS up to 30% positively affects the strength evolution of GB. The main reaction product of FA/EAFS blends was amorphous N–(C)–A–S–H gel along with geopolymer-type gel (N–A–S–H). Thermal resistance of GB was considered from the standpoint of their mechanical and dimensional stability after heating in the temperature interval of 600–800 °C. The changes in mechanical and thermal properties of GB after heating are attributed to the changes in their structure. The results have shown that EAFS negatively affects the thermal resistance of GB above 600 °C due to the phase transition and morphological transformation of the amorphous gel phase