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Erschienen in: Journal of Sol-Gel Science and Technology 3/2017

27.03.2017 | Original Paper: Fundamentals of sol-gel and hybrid materials processing

Production of cerium dioxide microspheres by an internal gelation sol–gel method

verfasst von: Jeffrey A. Katalenich

Erschienen in: Journal of Sol-Gel Science and Technology | Ausgabe 3/2017

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Abstract

An internal gelation sol–gel technique was used to prepare cerium dioxide microspheres with uniform diameters near 100 µm. In this process, chilled aqueous solutions containing cerium, hexamethylenetetramine (HMTA), and urea are transformed into a solid gel by heat addition and are subsequently washed, dried, and sintered to produce pure cerium dioxide. Cerous nitrate and ceric ammonium nitrate solutions were compared for their usefulness in microsphere production. Gelation experiments were performed with both cerous nitrate and ceric ammonium nitrate to determine desirable concentrations of cerium, HMTA, and urea in feed solutions as well as the necessary quantity of ammonium hydroxide added to cerium solutions. Analysis of the pH before and after sample gelation was found to provide a quantitative metric for optimal parameter selection along with subjective evaluations of gel qualities. The time necessary for chilled solutions to gel upon inserting into a hot water bath was determined for samples with a variety of parameters and also used to determine desirable formulations for microsphere production. A technique for choosing the optimal mixture of ceric ammonium nitrate, HMTA, and urea was determined using gelation experiments and used to produce microspheres by dispersion of the feed solution into heated silicone oil. Gelled spheres were washed to remove excess reactants and reaction products before being dried and sintered. X-ray diffraction of air-dried microspheres, sintered microspheres, and commercial CeO2 powders indicated that air-dried and sintered spheres were pure CeO2.

Graphical Abstract

https://static-content.springer.com/image/art%3A10.1007%2Fs10971-017-4345-8/MediaObjects/10971_2017_4345_Figa_HTML.gif

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Metadaten
Titel
Production of cerium dioxide microspheres by an internal gelation sol–gel method
verfasst von
Jeffrey A. Katalenich
Publikationsdatum
27.03.2017
Verlag
Springer US
Erschienen in
Journal of Sol-Gel Science and Technology / Ausgabe 3/2017
Print ISSN: 0928-0707
Elektronische ISSN: 1573-4846
DOI
https://doi.org/10.1007/s10971-017-4345-8

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