Preparation and characterization of zirconia and mixed zirconia/titania in ionic liquids

• Published in: Journal of materials science 2011-05, Vol.46 (10), p.3330-3336
• Main Authors: Farag, Hala K., Hegab, Khaled H., Zein El Abedin, S.
• Format: Article
• Language: English
• Subjects: Amides; Anatase; Characterization and Evaluation of Materials; Chemical properties; Chemistry and Materials Science; Classical Mechanics; Crystallography and Scattering Methods; Differential thermal analysis; Differential thermogravimetric analysis; Diffraction; Ionic liquids; Ions; Materials Science; Mixed oxides; Morphology; Nanorods; Phase transitions; Polymer Sciences; Powders; Scanning electron microscopy; Sol-gel processes; Solid Mechanics; Solvents; Synthesis; Titanium dioxide; Titanium dioxide-Zirconia; X-ray diffraction; X-rays; Zirconium; Zirconium dioxide; Zirconium oxide
• ISSN: 0022-2461; 1573-4803
• DOI: 10.1007/s10853-010-5220-y

Zirconia and mixed zirconia/titania were synthesized in two different ionic liquids, namely, 1-butyl-1-methylpyrrolidinium bis(trifluoromethylsulfonyl) amide ([BMP]TFSA) and 1-ethyl-3-methylimidazolium bis(trifluoromethylsulfonyl) amide ([EMIm]TFSA) using sol–gel methods. The synthesized oxides were characterized by means of X-ray diffraction, scanning electron microscopy with energy dispersive X-ray (SEM-EDX)), thermogravimetric and differential thermal analyses (TGA–DTA). The results show that the as-synthesized ZrO 2 powders obtained either in [BMP]TFSA or in [EMIm]TFSA show amorphous behaviour, and calcination at 500 °C yields t-ZrO 2 which is subject to further phase transformation to m-ZrO 2 at 1000 °C. The type of the ionic liquid influences the morphology of the synthesized zirconia as the sample obtained from [BMP]TFSA showed a porous morphology with very fine particles in the nanometer regime, whereas micro-rods were obtained from [EMIm]TFSA. ZrO 2 -TiO 2 nanorods with an average diameter of about 100 nm were synthesized in [EMIm]TFSA. The presence of zirconia in the mixed oxides stabilizes the anatase phase and elevates the temperature at which the phase transformation to rutile occurs.