Chlorination and Solvothermal Treatment of Zr(C₅H₅)₂Cl₂: a Synthetic Combination to Produce Nanometric Tetragonal ZrO₂

Abstract

A novel synthetic strategy based on the combination of the chlorination of an organometallic precursor followed by solvothermal treatment is found to be successful in the synthesis of tetragonal nano-ZrO(2) or nano-ZrO(2), embedded in an amorphous carbon matrix, depending on the solvent employed in the solvothermal step. The chemical and structural features (chemical composition, size and surface defects) of the intermediate and final materials have been determined experimentally mainly by high resolution transmission electron microscopy, electron energy loss spectroscopy, and Z-contrast images. These local techniques reveal that the nanoparticles consist of tetragonal ZrO(2) with an average size of 1.7 ± 0.4 and 6.2 ± 0.9 nm for the embedded in carbon and the free nano-ZrO(2), respectively.

Controllable synthesis of zirconia nano-powders using vapor-phase hydrolysis and theoretical analysis

“…Its interpretation allows us to determine the crystallographic phase if we compare our experimental ring pattern with those simulated for the cubic and tetragonal ZrO 2 polymorphs. 56 The clear pattern ts all the rings calculated for the tetragonal phase and some rings calculated for the cubic phase. So the particles are a mixture of tetragonal and cubic ZrO 2 , and we also nd that the content of the former is slightly higher than the latter.…”

Fabrication of Porous ZrO2 Nanostructures with Controlled Crystalline Phases and Structures via a Facile and Cost-Effective Hydrothermal Approach

“…Further microstructural information is obtained from HRTEM observation. A typical HRTEM image of the ZrO 2 -15 sample depicts the clear lattice fringes with an interplanar spacing of 0.296 nm for the (101) plane of the t -ZrO 2 phase (Figure d), while the SAED pattern indicates the discernible diffraction rings perfectly indexed to the same positions as those for the standard t -ZrO 2 phase …”

Sulfated Well-Defined Mesoporous Nanostructured Zirconia for Levulinic Acid Esterification

“…These distinctive properties make zirconia a good choice for a wide range of applications, such as solid fuel cells, ceramics, thermal barrier coating materials, catalysts, pigments, and luminescent materials or sensors when doped by rare earth elements. − These applications depend not only on the structural properties and crystallinity, particle size, and morphologies of zirconia but also on its porosity . Zirconia has been synthesized by various methods such as sol–gel process, − coprecipitation , hydrothermal or solvothermal synthesis, − pulsed plasma technique, aerosol pyrolysis, , and more recently, sustainable methods such as gelation of alginate, precipitation by hydroxypropyl-β-cyclodextrin, use of lysozyme, which is a cationic antibacterial enzyme, and use of Fusarium oxysporum , which is a species of plant parasitic fungus . The synthesis of mesoporous zirconia with narrow pore size distribution for specific applications has received ample attention. − Pârvulescu et al prepared mesoporous zirconia via a sol–gel procedure using ammonium salts as surfactants with linear alkyl chains wherein the effects of various parameters on the porous texture, especially ratios of the Zr/H 2 O and Zr/surfactant, were examined to establish their influence on the porous texture (surface area and pore size) .…”