The effect of the aging time of the ZrO2·nH2 O coagel: features of its phase formation and the evolution of its adsorption properties
Abstract
To date, researchers have failed to provide a physicochemical explanation of the crystallization of low-soluble X-ray amorphous ZrO2·nH2O caused by its aging in contact with the mother liquor. Data obtained in previous studies may be erroneous due to the unpredictable effect of Si4+, Na+ and K+ impurity ions. This study is aimed at establishing the regularities and features of the phase formation, as well as changes in the adsorption properties of ZrO2·nH2O and the functional composition of the ZrO2 surface depending on the aging time of the ZrO2·nH2O coagel in contact with the mother solution and in absence of impurity ions. The research was carried out on ZrO2·nH2O obtained by direct precipitation at pH = 10 followed by aging for 6–406 h in a fluoroplastic reactor and on ZrO2 obtained by heat treatment of the corresponding ZrO2·nH2O at 500 °C.
The properties of ZrO2·nH2O and ZrO2 were studied by methods of synchronous thermal analysis, X-ray diffraction, scanning electron microscopy, low-temperature N2 sorption, vacuum infrared spectroscopy, infrared spectroscopy, and temperature programmed desorption of molecular probes. It was shown that there is an extremum of the phase composition and adsorption properties of ZrO2·nH2O and ZrO2 after 24–96 h of aging.
It was established for the first time that the process of decomposition of dense aggregates of primary particles and submicron and micron aggregates and agglomerates of X-ray amorphous ZrO2·nH2O accompanied by the appearance of edge OH-groups precedes its crystallization in contact with the mother solution (6–48 h). Further aging (96–406 h) revealed a gradual crystallization of ZrO2·nH2O in the form of a mixture of the tetragonal and monoclinic phases of ZrO2 in a 1:1 ratio as a result of the attachment of primary particles of ZrO2·nH2O with the participation of edge and bridging OH groups. Acid-base properties of the ZrO2 surface are in extreme dependence on the aging time. With prolonged aging (more than 213 hours), the acid function of the ZrO2 surface begins to prevail due to the participation of the basic edge OH groups in the attachment of the ZrO2·nH2O primary particles. The observed changes are discussed from the perspective of the theory of oriented attachment of nanocrystals
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