Summary. In the present work, a study of H⁺ effects on the microstructure and morphology of hydroxyapatite synthesized by the hydrothermal method is reported. The synthesis was realized with pH values of 10, 9.6, 9, 8, and 7. To know the particle size distribution, growth habit, chemical composition, and crystalline phases present, SEM-EDS, XRD, AFM, and FTIR spectroscopy techniques were used and completed with Rietveld analysis. The obtained results showed an important effect of H⁺ on the morphological and crystallographic characteristics of the hydroxyapatite, demonstrating that the shape and nanoparticle size, as well as the number of crystalline phases, can change depending on the pH during the synthesis. It was observed that there is an increase in the formation of the monoclinic phase and a decrease of the hexagonal phase when the pH value diminishes from 9.6 to 7. The crystallite size also decreases from 46.69 to 19.56nm. An explanation of the role of pH on the final characteristics of the hydroxyapatite was related to the amount of H⁺ and OH^- ions, and it was included in this work.

Hydroxyapatite (HAp) is a natural hard tissue constituent widely used for bone and tooth replacement engineering. In the present work, synthetic HAp was obtained from calcium nitrate tetrahydrate (Ca(NO₃)₂·4H₂O) and ammonium phosphate dibasic (NH₄)₂HPO₄ following an optimized microwave assisted hydrothermal method. The effect of pH was evaluated by the addition of ammonium hydroxide (NH₄OH). Hence, different characterization techniques were used to determine its influence on the resulted HAp powders’ size, shape, and crystallinity. By Transmission Electron Microscopy (TEM), it was observed that the reaction pH environment modifies the morphology of HAp, and a shape evolution, from sub-hedral particles at pH = 7 to rod-like nanosized HAp at pH = 10, was confirmed. Using the X-ray Diffraction (XRD) technique, the characteristic diffraction peaks of the monoclinic phase were identified. Even if the performed Rietveld analysis indicated the presence of both phases (hexagonal and monoclinic), monoclinic HAp prevails in 95% with an average crystallite size of about 23 nm. The infrared spectra (FTIR) showed absorption bands at 3468 cm⁻¹ and 630 cm⁻¹ associated with OH⁻ of hydroxyapatite, and bands at 584 cm⁻¹, 960 cm⁻¹, and 1090 cm⁻¹ that correspond to the PO₄³⁻ and CO₃²⁻ characteristic groups. In summary, this work contributes to obtaining nanosized rod-like monoclinic HAp by a simple and soft method that has not been previously reported.

The goal of this work was to analyse ZrO(2) in the pure state and when doped with Ag nanoparticles, by electron microscopy, x-ray diffraction and thermoluminescence methods. According to the results obtained, Ag nanoparticles did not modify the morphology or the crystalline structure of the ZrO(2). The thermoluminescent (TL) response of pure ZrO(2) showed two peaks, one at 334 K and the other at 417 K, when it was exposed to ultraviolet (UV) radiation, and at 342 and 397 K when gamma radiation was used. For ZrO(2) impregnated with Ag nanoparticles a diminished TL intensity due to nanoparticle shielding was observed, but the glow curve shape was similar. However, when Ag nanoparticles were added during the ZrO(2) synthesis, a shift of the TL peaks towards higher temperature values with reference to pure ZrO(2) was observed. A linear dependence of the integrated TL signal as a function of the irradiation dose was observed in all analysed samples. It was possible to determine some kinetic parameters, such as activation energy, kinetic order and frequency factor, using the sequential quadratic programming glow curve deconvolution; it was found that these values are highly dependent on the type of radiation used. Ag nanoparticles present in ZrO(2) also modified the kinetic parameters, mainly when they were added during the synthesis of ZrO(2). Our results reinforce the possibilities of using pure and doped ZrO(2) as an appropriate dosimetric material in radiation physics.

Silver nanowires were used as templates to synthesize silver-doped CeO₂ (Ag–CeO₂ ) nanotubes by the precipitation method. The precipitated solid was dried at 100 °C for 24 h and calcined at 500 °C for 5 h. A TEM, HRTEM, LV-SEM and XRD study was carried out to determine the micro and nanostructural characteristics of the samples. LV-SEM analysis allowed us to observe microtubular empty structures constituted by Ce, O and Ag as indicated by EDS. These tubular structures, with an external diameter from 120 to 280 nm and an internal diameter from 40 to 80 nm, were mainly composed of 11 nm ceria nanoparticles. This kind of structures was obtained when CeO₂ nanoparticles covered the Ag nanowires during the synthesis. Due to the presence of ammonium hydroxide used during the synthesis, a fraction of the silver nanowire reacts and Ag atoms begin to migrate outside the ceria microtube. When the sintering process is applied, the Kirkendall effect can occur. So, out-diffusion of the remnant Ag through the interface is faster than the in-diffusion of the shell material (CeO₂ ), which eventually results in a coaxial nanotube on completion of the non-equilibrium interdiffusion, leaving the central core completely empty, driving the formation of hollow tubular Ag–CeO₂ structures as a result.

Structural and morphological properties of hydronium-potassium jarosite microstructures were investigated in this work, and their electrical properties were evaluated. All the microstructures were synthesized at a very low temperature of 70 °C with a reduced reaction time of 3 h. An increase in the pH from 0.8 to 2.1 decreased the particle sizes from 3 µm to 200 nm and an increase in the aging time from zero, three, and seven days resulted in semispherical, spherical, and euhedral jarosite structures, respectively. The Rietveld analysis also confirmed that the amount of hydronium substitution by potassium in the cationic site increased with an increase in pH. The percentages of hydronium jarosite (JH)/potassium jarosite (JK) for pH values of 0.8, 1.1, and 2.1 were 77.72/22.29%, 82.44/17.56%, and 89.98/10.02%, respectively. Microstructures obtained in this work were tested as alternative anode materials and the voltage measured using these electrodes made with hydronium-potassium jarosite microstructures and graphite ranged from 0.89 to 1.36 V. The results obtained in this work show that with reduced particle size and euhedral morphology obtained, modified jarosite microstructures can be used as anode materials for improving the lifetime of lithium-ion batteries.