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Synthesis of ZrO 2 Nanoparticles by Freeze Drying
Author(s) -
Tallón Carolina,
Moreno Rodrigo,
Nieto Ma Isabel
Publication year - 2009
Publication title -
international journal of applied ceramic technology
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.4
H-Index - 57
eISSN - 1744-7402
pISSN - 1546-542X
DOI - 10.1111/j.1744-7402.2008.02279.x
Subject(s) - materials science , agglomerate , cubic zirconia , sublimation (psychology) , nanoparticle , chemical engineering , monoclinic crystal system , acicular , thermal treatment , porosity , sonication , transmission electron microscopy , economies of agglomeration , particle size , specific surface area , phase (matter) , nanotechnology , microstructure , composite material , crystallography , crystal structure , organic chemistry , ceramic , psychology , chemistry , engineering , psychotherapist , catalysis
The interest in zirconia nanoparticles for either structural or functional applications depending on the stabilized phases has promoted the search for different synthesis methods. One of these methods is freeze drying. The present work deals with the preparation of zirconia nanoparticles by freeze drying using ZrOCl 2 solutions. The freeze‐dried powders consist of nonspherical granules made up of soft agglomerates of ZrO 2 with a d BET down to 40 nm and specific surface area values of 2–27 m 2 /depending on the thermal treatment. Granules have a low remaining porosity formed as a consequence of the sublimation of ice. The thermal treatment determined the crystalline phase formed, and so a study of the phase transformations with temperature has been carried out by X‐ray diffraction and transmission electron microscopy. The results indicate that at temperatures ≤400°C and a short duration of treatment, t ‐ZrO 2 is obtained with an acicular shape, while higher temperatures lead to the transformation into a monoclinic phase, which is accomplished by grain size growth, larger aspect ratio, and increased agglomeration. After sonication of the diluted suspensions, monomodal particle size distributions are obtained, with average sizes of ≅100 nm, thus demonstrating that agglomerates are soft and can be easily broken down.