Structural insights of mechanically induced aluminum-doped hydroxyapatite nanoparticles by Rietveld refinement

Aluminum doped hydroxyapatite(HA:Al^(3+)) nanopowders were successfully prepared via a simple and efficient one-pot mechanochemical route. The effects of dopant loading on phase compositions and structural features were assessed by Rietveld analysis. The XRD-Rietveld refinement revealed the stabilization of HA in hexagonal structure for all the samples. The sharpness and intensity of the apatite-derived XRD peaks decreased as the dopant content increased to 10% due to the increase in lattice imperfections and mechanically induced amorphization. The incorporation of Al3+into the HA lattice decreased the unit cell parameters. From the FTIR measurements, the representing bands of apatite were identified in all cases. The mechanosynthesized nanopowders consisted of nanospheroids with an average size of 44 ± 20 nm and therefore are promising for bone tissue regeneration.

Structural Characterization of Nanocrystalline Ni_(50-x)Ti₅₀Cu_x(X = 5, 9 wt%) Alloys Produced by Mechanical Alloying

Nanocrystalline Ni(50-x)Ti50Cux(X = 5, 9 wt%) alloys were successfully produced by mechanical alloying. Mechanical activation was performed at different milling times under a high purity argon (99.998 vol%) atmosphere. Phase analysis and structural features of the samples were examined by X-ray diffraction (XRD). Results revealed that NiTiCu (B2) phase was achieved after 600 min of milling. The formation of this phase was mostly related to the critical factors in determining the site replacement of elements in Ni-Ti-Cu ternary system. After 600 min of milling, the average crystallite size and lattice strain of the samples were about 5 - 10 nm and 1.057% - 1.967%, respectively. Evaluation of the full width at half maximum (FWHM) values for all the samples indicated the occurrence of anisotropic line broadening. The determined amounts of crystallinity revealed that the fraction of crystalline phase decreased with increasing weight percentage of copper up to 9% and reached a minimum value after 600 min of milling. The lattice parameters and the unit cell volume of the milled samples were always larger than the standard values. In addition, lattice parameter deviation influenced by the weight percentage of copper. Based on the obtained data, mechanical alloying process can be used for production of nanocrystalline NiTiCu alloys with different structural features.

Characterization of single-crystal fluorapatite nanoparticles synthesized via mechanochemical method

The synthesis of nanostructured fiuorapatite （FA; Calo（PO4）6F2） was explored from the starting materials of CaHPO4, Ca（OH）2, CaO, P205 and CaF2 via a mechanochemical process. In this research, the suitability of using the mechanochemical process to prepare a high crystalline phase of FA was studied. The characterization and structural features of the synthesized powders were evaluated using powder X-ray diffraction （XRD）, Fourier transform infrared spectroscopy （FT-IR）, energy dispersive X-ray spectroscopy （EDX）, scanning electron microscopy （SEM）, and transmission electron microscopy （TEM） techniques. The results from the structural studies indicate that the maximum lattice disturbance in the apatite structure after the mechanochemical process was at the （0 0 2） plane. Furthermore, the maximum particle size was below the crystallite size after 60 h of milling and subsequent thermal treatment at 600 ℃ for 1 h （heated up to 600 ℃ and kept for 1 h at this temperature）. We determined that this method gives rise to the single-crystal FA with an average size in the range of 25 ± 5 to 29 ± 9 rim. The present findings suggest that the solid-state reaction and appropriate thermal process simultaneously lead to the formation of nanostructured FA with spheroidal shape.

Thermal treatment effect on structural features of mechano-synthesized fluorapatite-titania nanocomposite: A comparative study

The influence of thermal treatment on the structural features of mechano-synthesized fluorapatite-titania composite nanopowders was studied.A mixture of calcium and phosphate reagents was mixed with a certain amount of titania(20 wt%)and then was mechanically activated for 5 h,10 h and 15 h respectively.After that,the mechano-synthesized powders were annealed at 700℃for 2 h.The crystallite size of the composite nanopowders estimated from Williamson-Hall method was in good agreement with transmission electron microscopy(TEM)analysis.Scanning electron microscopy(SEM)/TEM images confirmed the formation of a cluster-like composite which was composed of ellipse-like nanoparticles with an average size of about 16±7 nm after 15 h of milling.During the milling process,large variations in mechanochemical behavior of the CaHPO_(4)-Ca(OH)_(2)-CaF2-TiO_(2) system were detected.After the beginning of milling,no trace of the composite was found due to the lack of sufficient time for the mechanical activation.When the mechanical activation time increased to 15 h,composite nanopowders with the crystallite size of around 21.66 nm were formed.During heating at 700℃,the recovery of crystallinity occurred and the fraction of crystalline phase reached a maximum around 88.79%for the 10-h milled sample.Results indicated that the structural features of the composite were strongly influenced by the subsequent annealing.

Characterization of mechanothermal-synthesized hydroxyapatite-magnesium titanate composite nanopowders

Hydroxyapatite-magnesium titanate composite nanopowders have been developed using a mechanothermal process.Thermal treatment of the milled powders at 700℃resulted in the formation of HAp/MgTiO_(3)-MgO nanocomposite.X-ray diffraction(XRD),scanning electron microscopy(SEM),transmission electron microscopy(TEM),and energy dispersive X-ray spectroscopy(EDX)techniques were utilized to characterize the synthesized powders.The results revealed that the dominant phases after mechanical activation were hydroxyapatite,anatase(TiO_(2))and periclase(MgO);while after thermal annealing process at 700℃,hydroxyapatite along with geikielite(MgTiO_(3))and periclase(MgO)were the major phases.Based on the XRD analysis,the evaluation of structural features of the samples indicated that the average crystallite sizes of hydroxyapatite after 10 h of milling and subsequent thermal treatment at 700℃were about 21 nm and 34 nm,respectively.Microscopic observations illustrated that the synthesized powders contained large agglomerates which consisted of significantly finer particles with spheroidal morphology.It is concluded that the mechanothermal method can be used to produce hydroxyapatite-based nanocomposite with appropriate structural and morphological features.