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

  • Original Paper: Fundamentals of sol-gel and hybrid materials processing
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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.

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Acknowledgements

The author would like to thank Brian Kitchen, Bruce Pierson, and Dr. Marek Flaska of the University of Michigan Nuclear Engineering and Radiological Sciences Department for their useful ideas, input, and review during the course of this work. This research was conducted with government support under and awarded by DoD, Air Force Office of Scientific Research, National Defense Science and Engineering Graduate (NDSEG) Fellowship, 32 CFR 168a. This material is based on work supported by the National Science Foundation Graduate Research Fellowship under Grant No. DGE 1256260. Any opinion, findings, and conclusions or recommendations expressed in this material is that of the author and does not necessarily reflect the views of the National Science Foundation. This material is based on work supported by the Center for Space Nuclear Research (CSNR) under the Universities Space Research Association (USRA) Subcontract 06711-003. The USRA operates the CSNR for the Idaho National Laboratory. This research was supported by a research seed grant received from the Michigan Space Grant Consortium with matching funds from the University of Michigan Department of Nuclear Engineering and Radiological Sciences.

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  1. Jeffrey A. Katalenich

    Present address: Pacific Northwest National Laboratory, 3230 Innovation Blvd., MSIN K8-24, Richland, WA, 99354, USA

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  1. Department of Nuclear Engineering and Radiological Sciences, University of Michigan, 2355 Bonisteel Blvd., Ann Arbor, MI, 48109, USA

    Jeffrey A. Katalenich

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Correspondence to Jeffrey A. Katalenich.

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Katalenich, J.A. Production of cerium dioxide microspheres by an internal gelation sol–gel method. J Sol-Gel Sci Technol 82, 654–663 (2017). https://doi.org/10.1007/s10971-017-4345-8

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  • DOI: https://doi.org/10.1007/s10971-017-4345-8

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