No Arabic abstract
To investigate excess-hydrolysis of titanium alkoxides, TiO2 powders were fabricated from titanium-tetra-isopropoxide using 6:1 and 100:1 H2O:Ti (r) ratios. Powders were dried and fired at a range of temperatures ( up to 800 C). Hydroxylation and organic content in powders were characterised using ATR-FTIR, laser Raman microspectroscopy, and elemental microanalysis; surface area and pore size distribution were evaluated using N2 gas adsorption; phase composition was analysed using XRD and laser Raman microspectroscopy; and crystallite size was evaluated by XRD, TEM and SEM. Results showed near-complete hydrolysis in a predominantly aqueous medium (r = 100), resulting in precipitated crystalline powders exhibiting brookite and anatase, which begin to transform to rutile below 500 C. Powders precipitated in a predominantly organic medium (r = 6) underwent partial hydrolysis, were highly porous and exhibited an amorphous structure, with crystallisation of anatase occurring at 300 C and transformation to rutile beginning at 500 to 600C.
TiO$_2$ and WO$_3$ are two of the most important earth-abundant electronic materials with applications in countless industries. Recently alloys of WO$_3$ and TiO$_2$ have been investigated leading to improvements of key performance indicators for a variety of applications ranging from photo-electrochemical water splitting to electrochromic smart windows. These positive reports and the complexity of the ternary W-Ti-O phase diagram motivate a comprehensive experimental screening of this phase space. Using combinatorial thermal oxidation of solid solution W$_{1-x}$Ti$_{x}$ precursors combined with bulk and surface analysis mapping we investigate the oxide phase formation and surface passivation of tungsten titanium oxide in the entire compositional range from pure WO$_3$ to TiO$_2$. The system shows a remarkable structural transition from monoclinic over cubic to tetragonal symmetry with increasing Ti concentration. In addition, a strong Ti surface enrichment is observed for precursor Ti-concentrations in excess of 55 at.%, resulting in the formation of a protective rutile-structured TiO$_2$ surface layer. Despite the structural transitions, the optical properties of the oxide alloys remain largely unaltered demonstrating an independent control of multiple functional properties in W$_{1-x}$Ti$_{x}$O$_{n}$. The results from this study provide valuable guidelines for future development of W$_{1-x}$Ti$_{x}$O$_{n}$ for electronic and energy applications, but also novel engineering approaches for surface functionalization and additive manufacturing of Ti-based alloys.
Multiferroic (Bi1-xLaxFeO3)0.5(PbTiO3)0.5 ceramics was prepared from mechanical synthesized nanopowders. The XRD studies revealed the tetragonal structure and the tetragonality decreased with La content. Dielectric response of the compounds was found to contain three anomalies: 1) relaxor-like behavior due to lattice disorder (below 300 K); 2) dielectric permittivity maxima at~400 K attributed to the presence of oxygen vacancies; 3) grain boundary effect above 475 K. The Curie point at ~500 K was observed for the compound with x=0.5. The composition near the morphotropic boundary: (Bi0.8La0.2FeO3)0.5(PbTiO3)0.5 shoved the highest remnant magnetization. The irreversible magnetic properties of the (Bi1-xLaxFeO3)0.5(PbTiO3)0.5 compounds can be explained in terms of disorder induced spin-glass behavior due to random substitution of La or Pb ions for Bi sites. A sharp step in magnetization about 250 K is caused by the A-site distortion associated with tilts of FeO6 octahedra leading to modification of Fe-O-Fe angles and of antiferromagnetic coupling between magnetic Fe3+ moments.
The thermal vacuum treatment effect on the optical absorption spectra of the TiO2 nanopowders, both pure and coated by the Ni-B clasters with the original electroless method was investigated. It was observed that the thermal treatment of pure TiO2 nanopowders does not change their optical absorption spectrum while after the coating of these powder particles by the Ni-B clasters the thermal treatment results in the increase of the optical light absorption in the visual region of spectrum. This points to the possibility of the significant improvement of the photocatalist efficiency of TiO2 nanopowders coated by the Ni-B clasters using the thermal treatment.
The preparation in thin film form of the known icosahedral phase in Ti-Ni-Zr bulk alloys has been investigated as a function of substrate temperature. Films were deposited by Pulsed Laser Deposition on sapphire substrates at temperatures ranging from room temperature to 350$^circ$C. Morphological and structural modifications have been followed by grazing incidence and $theta$-2$theta$ X-ray diffraction, transmission electron diffraction and imaging. Chemical composition has been analysed by Electron Probe Micro-Analysis. The in-depth variation of composition has been studied by Secondary Neutral Mass Spectroscopy. We show that Pulsed Laser Deposition at 275$^circ$C makes the formation of a 1 m thick film of Ti-Ni-Zr quasicrystalline textured nanocrystallites possible.
Single-domain particles of SrFe8Al4O19 were prepared by thermal treatment at 1473 K of porous products of citrate-nitrate auto-combustion, and the influence of synthesis time on the particle morphology and magnetic properties was studied. The procedure allows to obtain SrFe8Al4O19 particles with mean diameters 100 - 460 nm, and their coercivity ranges from 14.5 to 18.4 kOe, while ferromagnetic resonance frequencies vary from 149 to 164 GHz.