Abstract
Nonhydrolytic sol-gel route is a relatively recent process which enables production of complex, multicomponent oxide materials. This process has some advantages over the conventional hydrolytic sol-gel route due to the ability to produce low-shrinkage, homogeneous, multicomponent gels. The objective of this work was to determine the effects of aging of nonhydrolytic gels on the composition, yield, phase transformations and morphology. Xerogels were prepared from aluminum chloride and isopropyl ether. Properties were studied using AgNO3 titrations, TGA/DTA, XRD, and BET analysis. We have found that the gels contain significant amount of chlorine where the Cl/Al atomic ratio ranges from 1.1–0.6 depending on the aging time. The crystallization temperature and enthalpy of crystallization decreased with aging time. The decrease of the surface area near the crystallization temperature correlates well with the decrease of the enthalpy of crystallization as a function of aging time. A closed pore phenomenon has been observed in the nonhydrolytic alumina system. Finally, analysis of the condensation degree (CD) yielding Al–O–Al bonds suggests that the rate determining step before the gel point is the alkoxy groups formation. However, during aging of the gels, the CD remains constant since the condensation of chloride with isopropoxy groups is stericly inhibited. Surface areas in the 300–650 m2/g range were obtained depending on the aging time.
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Grader, G., de Hazan, Y., Bravo-Zhivotovskii, D. et al. Effect of Aging on Nonhydrolytic Alumina Xerogels. Journal of Sol-Gel Science and Technology 10, 127–137 (1997). https://doi.org/10.1023/A:1018391311997
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DOI: https://doi.org/10.1023/A:1018391311997